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414 values
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36
36
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4
873
rxn_insight_reaction
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19
1.07k
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14
3.37k
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1
581
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1
433
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large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
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large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
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large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-69620ec491364bf69d7ad8a18f9b26bf
CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCO)CC1.Clc1nccnc1Cl>>CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCOc2nccnc2Cl)CC1
O.[H-].[Na+].C(C)(C)(C)OC(=O)N1CCN(CC1)C=1C(=NC=CN1)OCCO.ClC1=NC=CN=C1Cl>>ClC=1C(=NC=CN1)OCCOC=1C(=NC=CN1)N1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13][cH:14][cH:15][n:16][c:17]2[O:18][CH2:19][CH2:20][OH:21])[CH2:29][CH2:30]1.Cl[c:22]1[n:23][cH:24][cH:25][n:26][c:27]1[Cl:28]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13][cH:14][cH:15][n...
CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCO)CC1.Clc1nccnc1Cl
CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCOc2nccnc2Cl)CC1
null
null
O1CCOCC1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8088ac3623a2ee47f375f73ca665bec9cf80b1384463e6e2f03125aecbcea517
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1cnc(OCCOc2nccnc2N2CCNCC2)cn1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[Cl;D1;H0:7].[C:8]-[C:9]-[OH;D1;+0:10]>>[C:8]-[C:9]-[O;H0;D2;+0:10]-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[Cl;D1;H0:7]
61.2
[{"value": 61.0, "product": "ClC=1C(=NC=CN1)OCCOC=1C(=NC=CN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.2, "product": "ClC=1C(=NC=CN1)OCCOC=1C(=NC=CN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
8
HOUR
NaH (50% in mineral oil; 0.153 g, 3.50 mmol) was added to a stirred solution of 2-[3-(4-tert-butoxycarbonyl-1-piperazinyl)-2-pyrazinyloxy]ethanol (1.00 g, 3.08 mmol; prepared in Example 52, Step 2) and 2,3-dichloropyrazine (1.0 g, 6.71 mmol) in dioxane (10 mL). The reaction was stirred in a sealed tube at 100° C. overn...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cnccn1
c1cnccn1
C1C[NH]CC[NH]1.c1cnccn1.c1cnccn1
HCl
O1CCOCC1
100
8
CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCO)CC1.Clc1nccnc1Cl>O1CCOCC1>CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCOc2nccnc2Cl)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1c37d26045e8497b9cc63392d9a6114a
C[O-].OCCOc1cccnc1Br>>COc1ncccc1OCCO
BrC1=NC=CC=C1OCCO.C[O-].[Na+]>>OCCOC=1C(=NC=CC1)OC
[CH3:1][O-:2].Br[c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][OH:12]>>[CH3:1][O:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][OH:12]
C[O-].OCCOc1cccnc1Br
COc1ncccc1OCCO
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
600484490705932a09b3fac6538a42c6f3fc156ab44a4ea0bbd020dd3eafd6ff
51fd03eb6a688046e417b9ed09ea0e72062396d005af1318b9b5f376a97da959
c1ccncc1
Br-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[#8:5]):[c:6].[C;D1;H3:7]-[O-;H0;D1:8]>>[#8:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[O;H0;D2;+0:8]-[C;D1;H3:7]):[#7;a:2]:[c:3]
45
[{"value": 45.0, "product": "OCCOC=1C(=NC=CC1)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.7, "product": "OCCOC=1C(=NC=CC1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of the product obtained in Step 1 (2.33 g, 10.7 mmol) and NaOMe (0.634 mg, 11.8 mmol) in MeOH (50 mL) was refluxed overnight. The reaction mixture was filtered and concentrated. The residue was purified by column chromatography on silica, using CH2Cl2/MeOH/heptane (4:1:5) as eluent, to give 0.81 g (45%) of th...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Ether
c1ccncc1
c1ccncc1
c1ccncc1
Br-
CO
null
null
C[O-].OCCOc1cccnc1Br>CO>COc1ncccc1OCCO
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fe13deb2f8f244b88eeb50d6b6084223
C[C@@H]1CN(C(c2ccccc2)(c2ccccc2)c2ccccc2)CCN1.Clc1nccnc1Cl>>C[C@@H]1CNCCN1c1nccnc1Cl
C(Cl)(Cl)Cl.CCO.C[C@@H]1CN(CCN1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.ClC1=NC=CN=C1Cl.C(=O)([O-])[O-].[K+].[K+]>>ClC=1C(=NC=CN1)N1[C@@H](CNCC1)C
c1ccc(C(c2ccccc2)(c2ccccc2)[N:4]2[CH2:3][C@@H:2]([CH3:1])[NH:7][CH2:6][CH2:5]2)cc1.Cl[c:8]1[n:9][cH:10][cH:11][n:12][c:13]1[Cl:14]>>[CH3:1][C@@H:2]1[CH2:3][NH:4][CH2:5][CH2:6][N:7]1[c:8]1[n:9][cH:10][cH:11][n:12][c:13]1[Cl:14]
C[C@@H]1CN(C(c2ccccc2)(c2ccccc2)c2ccccc2)CCN1.Clc1nccnc1Cl
C[C@@H]1CNCCN1c1nccnc1Cl
null
null
O.CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
a9eb66e8dbd1d24aca814a8b35622449727e860aa374e764e270d6d462ef3f42
5c70578d0819c8a1731196f6e967b1ca081ac9fc97f879ecb5b3f5b29f334150
c1cnc(N2CCNCC2)cn1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[Cl;D1;H0:7].[C;D1;H3:8]-[C:9]1-[C:10]-[N;H0;D3;+0:11](-C(-c2:c:c:c:c:c:2)(-c2:c:c:c:c:c:2)-c2:c:c:c:c:c:2)-[C:12]-[C:13]-[NH;D2;+0:14]-1>>[C;D1;H3:8]-[C:9]1-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]-[N;H0;D3;+0:14]-1-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:...
66
[{"value": 66.0, "product": "ClC=1C(=NC=CN1)N1[C@@H](CNCC1)C", "details": "PERCENTYIELD", "is_desired": false}]
110
CELSIUS
30
MINUTE
A mixture of the product obtained in Step 1 above, 2,3-dichloropyrazine (154 g, 1.00 mmol) and K2CO3 (160 g, 1.20 mol) in DMF (1 L) was heated at 110° C. for 20 h with vigorous stirring. (TLC monitoring system: CHCl3: EtOH (20:1); silica). The mixture was cooled and poured slowly into water (6 L) with stirring. The sol...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine.Tertiary amine
Secondary amine.Tertiary amine
c1ccccc1.c1ccccc1.c1ccccc1.C1C[NH]CCN1.c1cnccn1
C1C[NH]CCN1.c1cnccn1
C1C[NH]CCN1.c1cnccn1
HCl
O.CN(C)C=O
110
0.5
C[C@@H]1CN(C(c2ccccc2)(c2ccccc2)c2ccccc2)CCN1.Clc1nccnc1Cl>O.CN(C)C=O>C[C@@H]1CNCCN1c1nccnc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-091c8811c9fa4cf69a2d9d1e364959ff
C[S-].OCCOc1cccnc1Cl>>CSc1ncccc1OCCO
C[S-].[Na+].ClC1=NC=CC=C1OCCO>>CSC1=NC=CC=C1OCCO
[CH3:1][S-:2].Cl[c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][OH:12]>>[CH3:1][S:2][c:3]1[n:4][cH:5][cH:6][cH:7][c:8]1[O:9][CH2:10][CH2:11][OH:12]
C[S-].OCCOc1cccnc1Cl
CSc1ncccc1OCCO
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
a043117f5ac6655ea3d4f71b77392fbb346566d5ecbe0b9ffd7138c05f760a35
1813ae14fbd9cacead4dcfaf9efbd2467a19b3e216836766b78aa6647dcfb48a
c1ccncc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[#8:5]):[c:6].[C;D1;H3:7]-[S-;H0;D1:8]>>[#8:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[S;H0;D2;+0:8]-[C;D1;H3:7]):[#7;a:2]:[c:3]
37.8
[{"value": 36.0, "product": "CSC1=NC=CC=C1OCCO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 37.8, "product": "CSC1=NC=CC=C1OCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a suspension of sodium thiomethoxide (3.01 g, 42.9 mmol) in dry DMF (30 mL) was 2-[(2-chloro-3-pyridinyl)oxy]ethanol (7.82 g, 45.1 mmol, from Example 193, Step 1) added and the reaction mixture was stirred at ambient temperature for 1 h. The solvent was removed under reduced pressure and the residue was partitioned ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Monosulfide
c1ccncc1
c1ccncc1
c1ccncc1
Other
CN(C)C=O
null
1
C[S-].OCCOc1cccnc1Cl>CN(C)C=O>CSc1ncccc1OCCO
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f1cb25eb303a4001b2704b07737cf170
CC(C)(C)[Si](C)(C)Cl.OCCOc1cccnc1Br>>CC(C)(C)[Si](C)(C)OCCOc1cccnc1Br
C[Si](C(C)(C)C)(C)Cl.BrC1=NC=CC=C1OCCO.N1C=NC=C1>>BrC1=NC=CC=C1OCCO[Si](C)(C)C(C)(C)C
Cl[Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([CH3:6])[CH3:7].[OH:8][CH2:9][CH2:10][O:11][c:12]1[cH:13][cH:14][cH:15][n:16][c:17]1[Br:18]>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:8][CH2:9][CH2:10][O:11][c:12]1[cH:13][cH:14][cH:15][n:16][c:17]1[Br:18]
CC(C)(C)[Si](C)(C)Cl.OCCOc1cccnc1Br
CC(C)(C)[Si](C)(C)OCCOc1cccnc1Br
null
null
CN(C)C=O.[OH-].[Na+]
Protection
Alcohol protection with silyl ethers
0085cd6629412592263fdf1537bdf8c19ef10dbeafe6f880807464d8107fa715
d2a170d01b2f3ec57d6fac058519475050ba5531f5d304635fb42e153d5bb9b5
c1ccncc1
Cl-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[C:8]-[C:9]-[OH;D1;+0:10]>>[C:8]-[C:9]-[O;H0;D2;+0:10]-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7]
null
[]
null
null
2
HOUR
A solution of dimethyl-t-butylsilyl chloride (11.1 g, 74 mmol) in DMF (30 mL) was added to a suspension of 2-bromo-3-(2-hydroxyethoxy)pyridine (15.3 g, 70 mmol; obtained in Example 191, Step 1) and imidazole (10.0 g, 147 mmol) in DMF (30 mL). The reaction mixture was stirred at ambient temperature for 2 h, diluted with...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Silyl protective group
TMS ether protective group
null
null
c1ccncc1
HCl
CN(C)C=O.[OH-].[Na+]
null
2
CC(C)(C)[Si](C)(C)Cl.OCCOc1cccnc1Br>CN(C)C=O.[OH-].[Na+]>CC(C)(C)[Si](C)(C)OCCOc1cccnc1Br
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-31743a51b6504dc4aba84a0f0347480d
CC(C)(C)[Si](C)(C)OCCOc1cccnc1Br.CCO>>CCOc1ncccc1OCCO
BrC1=NC=CC=C1OCCO[Si](C)(C)C(C)(C)C.[O-]CC.[Na+].CCO>>C(C)OC1=NC=CC=C1OCCO
CC(C)(C)[Si](C)(C)[O:13][CH2:12][CH2:11][O:10][c:9]1[c:4](Br)[n:5][cH:6][cH:7][cH:8]1.[CH3:1][CH2:2][OH:3]>>[CH3:1][CH2:2][O:3][c:4]1[n:5][cH:6][cH:7][cH:8][c:9]1[O:10][CH2:11][CH2:12][OH:13]
CC(C)(C)[Si](C)(C)OCCOc1cccnc1Br.CCO
CCOc1ncccc1OCCO
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
f117966458f382029b157cde8b0bf9401f9660eea179a83a9a7113216473521f
f216e281e35fe518b2085df6af208cbe54ed366b8463456b519ba975028ae7ec
c1ccncc1
Br-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[#8:5]-[C:6]-[C:7]-[O;H0;D2;+0:8]-[Si](-C)(-C)-C(-C)(-C)-C):[c:9].[C;D1;H3:10]-[C:11]-[OH;D1;+0:12]>>[C;D1;H3:10]-[C:11]-[O;H0;D2;+0:12]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[c:4](-[#8:5]-[C:6]-[C:7]-[OH;D1;+0:8]):[c:9]
41
[{"value": 41.0, "product": "C(C)OC1=NC=CC=C1OCCO", "details": "PERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
The product obtained in Step 1 above (13.2 g, 39.7 mmol) was added to sodium ethoxide in EtOH [prepared from Na (10.5 g, 457 mmol) and EtOH (200 mL)]. The resulting mixture was heated at 70° C. overnight. After cooling to ambient temperature, the reaction mixture was diluted with ice water (0.8 L) and extracted with Et...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol.TMS ether protective group
Ether.Primary alcohol
c1ccncc1
c1ccncc1
c1ccncc1
HBr
null
70
null
CC(C)(C)[Si](C)(C)OCCOc1cccnc1Br.CCO>>CCOc1ncccc1OCCO
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d018fec252db4e5a9e88142adb2f4a73
C=O.COc1ccc(N)cc1O>>COc1ccc(N(C)C)cc1O
[H-].NC=1C=CC(=C(C1)O)OC.C=O.C(#N)[BH3-].[Na+]>>CN(C=1C=CC(=C(C1)O)OC)C
O=[CH2:8].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([NH2:7])[cH:10][c:11]1[OH:12]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([N:7]([CH3:8])[CH3:9])[cH:10][c:11]1[OH:12]
C=O.COc1ccc(N)cc1O
COc1ccc(N(C)C)cc1O
null
null
C(C)(=O)O.C(C)O
Heteroatom Alkylation and Arylation
Eschweiler-Clarke Primary Amine Methylation
5bc40be4d4b4346801fbfcec480fec37de3ff2eecebe2990b3686fa4792d12b6
5cdbf447f632627824e84e0bcac2293ea9ebd70c19b0d56dea90691653b444c7
c1ccccc1
O=[CH2;D1;+0:1].[NH2;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[C;D1;H3:6]-[N;H0;D3;+0:2](-[CH3;D1;+0:1])-[c:3](:[c:4]):[c:5]
20
[{"value": 20.0, "product": "CN(C=1C=CC(=C(C1)O)OC)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a stirred solution of 5-amino-2-methoxyphenol (5.0 g, 36 mmol) in ethanol (250 mL), was added 33% formaldehyde (4×1.5 mL at times 0, 60 min, 140 min and 185 min) and sodium cyanoborohydride (4×0.8 g, at times 30 min, 120 min, 165 min and 210 min). After each addition of the hydride, pH was adjusted to ˜6 using aceti...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde.Primary amine
Tertiary amine
null
null
c1ccccc1
null
C(C)(=O)O.C(C)O
null
2
C=O.COc1ccc(N)cc1O>C(C)(=O)O.C(C)O>COc1ccc(N(C)C)cc1O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3555db0f151642c7b45cc764313fca0f
C1CNCCN1.Clc1nsnc1Cl>>Cl.Clc1nsnc1N1CCNCC1
ClC1=NSN=C1Cl.O.O.O.O.O.O.N1CCNCC1.[OH-].[Na+]>>Cl.ClC1=NSN=C1N1CCNCC1
[NH:8]1[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1.[Cl:1][c:7]1[c:3]([Cl:2])[n:4][s:5][n:6]1>>[ClH:1].[Cl:2][c:3]1[n:4][s:5][n:6][c:7]1[N:8]1[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1
C1CNCCN1.Clc1nsnc1Cl
Cl.Clc1nsnc1N1CCNCC1
null
null
[Cl-].[Na+].O.CN(C)C=O
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
adffb830a4483326d742b7dc1e45dc4b03e33fa8db2a297e07883f222e2c68d3
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1nsnc1N1CCNCC1
[#7:1]1-[C:2]-[C:3]-[NH;D2;+0:4]-[C:5]-[C:6]-1.[Cl;D1;H0:7]-[c:8]1:[#7;a:9]:[#16;a:10]:[#7;a:11]:[c;H0;D3;+0:12]:1-[Cl;H0;D1;+0:13]>>[Cl;D1;H0:7]-[c:8]1:[#7;a:9]:[#16;a:10]:[#7;a:11]:[c;H0;D3;+0:12]:1-[N;H0;D3;+0:4]1-[C:5]-[C:6]-[#7:1]-[C:2]-[C:3]-1.[ClH;D0;+0:13]
89
[{"value": 52.0, "product": "Cl.ClC1=NSN=C1N1CCNCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.0, "product": "Cl.ClC1=NSN=C1N1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
null
null
A mixture of 3,4-dichloro-1,2,5-thiadiazole (4.00 g, 25.8 mmol) and piperazine hexahydrate (25.0 g, 130 mmol) in DMF (25 mL) was heated at 70° C. for 20 minutes. After cooling to ambient temperature, the reaction mixture was basified (11M NaOH) and brine was added. The resulting mixture was extracted with CHCl3 (×3). T...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1CNCCN1.c1cnsn1
c1cnsn1.C1C[NH]CCN1
c1cnsn1.C1C[NH]CCN1
null
[Cl-].[Na+].O.CN(C)C=O
70
null
C1CNCCN1.Clc1nsnc1Cl>[Cl-].[Na+].O.CN(C)C=O>Cl.Clc1nsnc1N1CCNCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ce211c22d47645f9b378ccf64f84926e
CC(C)(C)OC(=O)N1CCN(c2nccnc2Cl)CC1.OCCS>>CC(C)(C)OC(=O)N1CCN(c2nccnc2SCCO)CC1
[OH-].[Na+].SCCO.ClC1=NC=CN=C1N1CCN(CC1)C(=O)OC(C)(C)C>>OCCSC=1C(=NC=CN1)N1CCN(CC1)C(=O)OC(C)(C)C
Cl[c:17]1[c:12]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:23][CH2:22]2)[n:13][cH:14][cH:15][n:16]1.[SH:18][CH2:19][CH2:20][OH:21]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13][cH:14][cH:15][n:16][c:17]2[S:18][CH2:19][CH2:20][OH:21])[CH...
CC(C)(C)OC(=O)N1CCN(c2nccnc2Cl)CC1.OCCS
CC(C)(C)OC(=O)N1CCN(c2nccnc2SCCO)CC1
null
null
O1CCOCC1.O
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution thiol
ceff1a344f68f64f3ccbdc170e0e8518aee636d7d51efddd7ec4c746a215b670
b7fe376f7aad2517725eef26ab981e4baa6c31c5f38fdf89e7c52a4a2c6cc1d2
c1cnc(N2CCNCC2)cn1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[#7:7].[C:8]-[C:9]-[SH;D1;+0:10]>>[#7:7]-[c:6]1:[#7;a:5]:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:1-[S;H0;D2;+0:10]-[C:9]-[C:8]
65.2
[{"value": 65.0, "product": "OCCSC=1C(=NC=CN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.2, "product": "OCCSC=1C(=NC=CN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
Sodium hydroxide (0.92 g, 23 mmol) was dissolved in water (9 mL) and dioxane (15 mL). 2-Mercaptoethanol (0.54 mL, 7.7 mmol) was added while stirring and 2-chloro-3-(4-tert-butoxycarbonyl-1-piperazinyl)pyrazine (2.3 g, 7.7 mmol, from Example 52, step 1) in dioxane (10 mL) was added. The reaction mixture was heated at 10...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aliphatic thiol
Monosulfide
c1cnccn1
c1cnccn1
C1C[NH]CC[NH]1.c1cnccn1
HCl
O1CCOCC1.O
100
null
CC(C)(C)OC(=O)N1CCN(c2nccnc2Cl)CC1.OCCS>O1CCOCC1.O>CC(C)(C)OC(=O)N1CCN(c2nccnc2SCCO)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-51b277b3a8fa4880acb62b1176d21922
CC(C)(C)OC(=O)N1CCNCC1.Clc1nsnc1Cl>>CC(C)(C)OC(=O)N1CCN(c2nsnc2Cl)CC1
C(=O)(OC(C)(C)C)N1CCNCC1.C(=O)([O-])[O-].[K+].[K+].ClC1=NSN=C1Cl>>ClC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][NH:11][CH2:18][CH2:19]1.Cl[c:12]1[n:13][s:14][n:15][c:16]1[Cl:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13][s:14][n:15][c:16]2[Cl:17])[CH2:18][CH2:19]1
CC(C)(C)OC(=O)N1CCNCC1.Clc1nsnc1Cl
CC(C)(C)OC(=O)N1CCN(c2nsnc2Cl)CC1
null
null
O.CC#N.CCOC(=O)C
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
3991cfe8cc7ce136c577c51c08d126d93c8ef536de9d097cdf4a1fb2a87bf134
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1nsnc1N1CCNCC1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[#16;a:3]:[#7;a:4]:[c:5]:1-[Cl;D1;H0:6].[#7:7]1-[C:8]-[C:9]-[NH;D2;+0:10]-[C:11]-[C:12]-1>>[Cl;D1;H0:6]-[c:5]1:[#7;a:4]:[#16;a:3]:[#7;a:2]:[c;H0;D3;+0:1]:1-[N;H0;D3;+0:10]1-[C:11]-[C:12]-[#7:7]-[C:8]-[C:9]-1
null
[]
100
CELSIUS
4
DAY
A mixture of N-Boc-piperazine (2.97 g, 15.9 mmol), K2CO3 (2.20 g, 15.9 mmol) and 3,4-dichloro-1,2,5-thiadiazole (1.5 mL, 15.9 mmol) in CH3CN (30 mL) was stirred at 100° C. for 19 h and at room temperature for 4 days. The reaction mixture was then diluted with EtOAc and water. The organic phase was dried (K2CO3) and the...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1C[NH]CCN1.c1cnsn1
C1C[NH]CC[NH]1.c1cnsn1
C1C[NH]CC[NH]1.c1cnsn1
HCl
O.CC#N.CCOC(=O)C
100
96
CC(C)(C)OC(=O)N1CCNCC1.Clc1nsnc1Cl>O.CC#N.CCOC(=O)C>CC(C)(C)OC(=O)N1CCN(c2nsnc2Cl)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-401e75184394424a991e98a2894f3ddc
CC(C)(C)OC(=O)N1CCN(c2nsnc2Cl)CC1.OCCO>>CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1
ClC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C.C(CO)O>>OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C
Cl[c:16]1[c:12]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:22][CH2:21]2)[n:13][s:14][n:15]1.[OH:17][CH2:18][CH2:19][OH:20]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13][s:14][n:15][c:16]2[O:17][CH2:18][CH2:19][OH:20])[CH2:21][CH2:22]1
CC(C)(C)OC(=O)N1CCN(c2nsnc2Cl)CC1.OCCO
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1
null
null
N1=CC=CC=C1.CCOC(=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
85f3a5bcedc3a3ca57fcccc5a225fd51bca5e111eec8d9d55c821c209d5319b1
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1nsnc1N1CCNCC1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[#16;a:3]:[#7;a:4]:[c:5]:1-[#7:6].[C:7]-[C:8]-[OH;D1;+0:9]>>[#7:6]-[c:5]1:[#7;a:4]:[#16;a:3]:[#7;a:2]:[c;H0;D3;+0:1]:1-[O;H0;D2;+0:9]-[C:8]-[C:7]
79.6
[{"value": 65.0, "product": "OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 79.6, "product": "OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
8
HOUR
K-t-BuO (1.24 g, 1 mmol) was added to a mixture of the product obtained in Step 1 (198 g, 6.5 mmol) and ethylene glycol (2.54 ml, 45.5 mmol) in pyridine (15 ml). The reaction mixture was stirred at 100° C. for 6 h and at room temperature overnight. The solution was then poured into ice-water and diluted with EtOAc. The...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cnsn1
c1cnsn1
C1C[NH]CC[NH]1.c1cnsn1
HCl
N1=CC=CC=C1.CCOC(=O)C
100
8
CC(C)(C)OC(=O)N1CCN(c2nsnc2Cl)CC1.OCCO>N1=CC=CC=C1.CCOC(=O)C>CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-98b19d8ee6d64b53b83dce7acbe77625
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1.O=c1ccc2ccc(O)cc2o1>>CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccc(=O)oc3c2)CC1
OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.OC1=CC=C2C=CC(OC2=C1)=O.N(=NC(=O)OCC)C(=O)OCC>>O=C1OC2=CC(=CC=C2C=C1)OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C
O[CH2:19][CH2:18][O:17][c:16]1[c:12]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:33][CH2:32]2)[n:13][s:14][n:15]1.[OH:20][c:21]1[cH:22][cH:23][c:24]2[cH:25][cH:26][c:27](=[O:28])[o:29][c:30]2[cH:31]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12...
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1.O=c1ccc2ccc(O)cc2o1
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccc(=O)oc3c2)CC1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
86bfb73617450d22f9456ed5ce4d96a73f1f8fc0c016bebae57fda68e2da86a2
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
O=c1ccc2ccc(OCCOc3nsnc3N3CCNCC3)cc2o1
O-[CH2;D2;+0:1]-[C:2]-[#8:3].[#8;a:4]:[c:5]:[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:8]-[c:7](:[c:9]):[c:6]:[c:5]:[#8;a:4]
123.6
[{"value": 123.6, "product": "O=C1OC2=CC(=CC=C2C=C1)OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
DAY
Diethyl azodicarboxylate (DEAD, 61 μl, 0.39 mmol) was added drop wise to a mixture of the product obtained in Step 2 (100 mg, 0.30 mmol), triphenylphosphine (102 mg, 0.39 mmol) and 7-hydroxycoumarin (63 mg, 0.39 mmol) in dry THF (5 mL). The reaction mixture was stirred at room temperature for 5 days. After solvent remo...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
null
C1C[NH]CC[NH]1.c1cnsn1.c1ccc2cccoc2c1
HO-
C1CCOC1
null
120
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1.O=c1ccc2ccc(O)cc2o1>C1CCOC1>CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccc(=O)oc3c2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8e8efdfb6a344bea937cd950ad54cd50
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccc(=O)oc3c2)CC1>>O=c1ccc2ccc(OCCOc3nsnc3N3CCNCC3)cc2o1
O=C1OC2=CC(=CC=C2C=C1)OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C.FC(C(=O)O)(F)F>>N1(CCNCC1)C=1C(=NSN1)OCCOC1=CC=C2C=CC(OC2=C1)=O
CC(C)(C)OC(=O)[N:21]1[CH2:20][CH2:19][N:18]([c:17]2[c:13]([O:12][CH2:11][CH2:10][O:9][c:8]3[cH:7][cH:6][c:5]4[cH:4][cH:3][c:2](=[O:1])[o:26][c:25]4[cH:24]3)[n:14][s:15][n:16]2)[CH2:23][CH2:22]1>>[O:1]=[c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][c:8]([O:9][CH2:10][CH2:11][O:12][c:13]3[n:14][s:15][n:16][c:17]3[N:18]3[CH2:19][CH...
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccc(=O)oc3c2)CC1
O=c1ccc2ccc(OCCOc3nsnc3N3CCNCC3)cc2o1
null
null
C(Cl)Cl
Reduction
Boc amine deprotection
2c25e19aee181a3c5131cfdfda27035fd54d4379a11d745dfb75d386bacfd500
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
O=c1ccc2ccc(OCCOc3nsnc3N3CCNCC3)cc2o1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1>>[#7:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-1
null
[]
0
CELSIUS
1
HOUR
The product obtained in Step 3 (176 mg) was diluted in CH2Cl2 (1.5 mL) and cooled to ˜0° C. Trifluoroacetic acid (0.5 mL) was added and the reaction mixture was stirred for 1 h at 5° C. After solvent removal in vacuo, the residue was purified by chromatography on silica gel using hexane/EtOAc (1:1) followed by CH2Cl2/M...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1C[NH]CC[NH]1
C1C[NH]CCN1
c1ccc2cccoc2c1.c1cnsn1.C1C[NH]CCN1
HO-
C(Cl)Cl
0
1
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccc(=O)oc3c2)CC1>C(Cl)Cl>O=c1ccc2ccc(OCCOc3nsnc3N3CCNCC3)cc2o1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b5614b95bb174987a2df04178fb2173e
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1.Oc1ccc2ccncc2c1>>CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccncc3c2)CC1
OC1=CC=C2C=CN=CC2=C1.OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C.N(=NC(=O)OCC)C(=O)OCC.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>C1=NC=CC2=CC=C(C=C12)OCCOC=1C(=NSN1)N1CCN(CC1)C(=O)OC(C)(C)C
O[CH2:19][CH2:18][O:17][c:16]1[c:12]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:32][CH2:31]2)[n:13][s:14][n:15]1.[OH:20][c:21]1[cH:22][cH:23][c:24]2[cH:25][cH:26][n:27][cH:28][c:29]2[cH:30]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13]...
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1.Oc1ccc2ccncc2c1
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccncc3c2)CC1
null
null
null
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether
86bfb73617450d22f9456ed5ce4d96a73f1f8fc0c016bebae57fda68e2da86a2
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1cc2ccc(OCCOc3nsnc3N3CCNCC3)cc2cn1
O-[CH2;D2;+0:1]-[C:2]-[#8:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
null
null
5
DAY
The title compound was prepared according to the procedure of Example 218, Step 3 starting from the product of Example 218, Step 2 (100 mg, 0.30 mmol), triphenylphosphine (102 mg, 0.39 mmol), 7-hydroxyisoquinoline (57 mg, 0.39 mmol) and diethyl azodicarboxylate (61 μl, 0.39 mmol) except that the reaction mixture was st...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
null
C1C[NH]CC[NH]1.c1cnsn1.c1ccc2cnccc2c1
HO-
null
null
120
CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCO)CC1.Oc1ccc2ccncc2c1>>CC(C)(C)OC(=O)N1CCN(c2nsnc2OCCOc2ccc3ccncc3c2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cc362952def14ec9ad18caceddb44035
CC(C)(C)OC(=O)N1CCN(c2nccnc2Cl)CC1.OCCOc1cccc(O)c1>>CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCOc2cccc(O)c2)CC1
ClC1=NC=CN=C1N1CCN(CC1)C(=O)OC(C)(C)C.OC=1C=C(OCCO)C=CC1.[H-].[Na+]>>OC=1C=C(OCCOC=2C(=NC=CN2)N2CCN(CC2)C(=O)OC(C)(C)C)C=CC1
Cl[c:17]1[c:12]([N:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:30][CH2:29]2)[n:13][cH:14][cH:15][n:16]1.[OH:18][CH2:19][CH2:20][O:21][c:22]1[cH:23][cH:24][cH:25][c:26]([OH:27])[cH:28]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][N:11]([c:12]2[n:13][cH:14][cH...
CC(C)(C)OC(=O)N1CCN(c2nccnc2Cl)CC1.OCCOc1cccc(O)c1
CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCOc2cccc(O)c2)CC1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8088ac3623a2ee47f375f73ca665bec9cf80b1384463e6e2f03125aecbcea517
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1ccc(OCCOc2nccnc2N2CCNCC2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[#7:7].[C:8]-[C:9]-[OH;D1;+0:10]>>[#7:7]-[c:6]1:[#7;a:5]:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:1-[O;H0;D2;+0:10]-[C:9]-[C:8]
94
[{"value": 94.0, "product": "OC=1C=C(OCCOC=2C(=NC=CN2)N2CCN(CC2)C(=O)OC(C)(C)C)C=CC1", "details": "PERCENTYIELD", "is_desired": false}]
65
CELSIUS
1.75
HOUR
To a stirred solution of 2-(3-hydroxyphenoxy)ethanol (7.71 g, 0.05 mol) in dry DMF to (100 mL) at ˜0° C. (ice bath) was added NaH (3.90 g, 0.163 mol) in portions under N2. When the H2-evolution had ceased, a solution of 2-chloro-3-(4-tert-butoxycarbonyl-1-piperazinyl)pyrazine (0.05 mol, 14.9 g; from Example 52, Step 1)...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cnccn1
c1cnccn1
C1C[NH]CC[NH]1.c1cnccn1.c1ccccc1
HCl
CN(C)C=O
65
1.75
CC(C)(C)OC(=O)N1CCN(c2nccnc2Cl)CC1.OCCOc1cccc(O)c1>CN(C)C=O>CC(C)(C)OC(=O)N1CCN(c2nccnc2OCCOc2cccc(O)c2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-87f51bec0164419d94ede3554fb73ac6
COCCOc1cccc(OCCOc2nccnc2N2CCN(C(=O)OC(C)(C)C)CC2)c1>>COCCOc1cccc(OCCOc2nccnc2N2CCNCC2)c1
COCCOC=1C=C(OCCOC=2C(=NC=CN2)N2CCN(CC2)C(=O)OC(C)(C)C)C=CC1>>COCCOC=1C=C(OCCOC2=NC=CN=C2N2CCNCC2)C=CC1
CC(C)(C)OC(=O)[N:24]1[CH2:23][CH2:22][N:21]([c:20]2[c:15]([O:14][CH2:13][CH2:12][O:11][c:10]3[cH:9][cH:8][cH:7][c:6]([O:5][CH2:4][CH2:3][O:2][CH3:1])[cH:27]3)[n:16][cH:17][cH:18][n:19]2)[CH2:26][CH2:25]1>>[CH3:1][O:2][CH2:3][CH2:4][O:5][c:6]1[cH:7][cH:8][cH:9][c:10]([O:11][CH2:12][CH2:13][O:14][c:15]2[n:16][cH:17][cH:1...
COCCOc1cccc(OCCOc2nccnc2N2CCN(C(=O)OC(C)(C)C)CC2)c1
COCCOc1cccc(OCCOc2nccnc2N2CCNCC2)c1
null
null
Cl.CCOCC.CCOCC.CCOC(=O)C
Reduction
Boc amine deprotection
2c25e19aee181a3c5131cfdfda27035fd54d4379a11d745dfb75d386bacfd500
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(OCCOc2nccnc2N2CCNCC2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1>>[#7:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:6]-[C:5]-1
69
[{"value": 69.0, "product": "COCCOC=1C=C(OCCOC2=NC=CN=C2N2CCNCC2)C=CC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
The product obtained in Step 1 above was dissolved in a mixture of EtOAc (18 mL) and ether (9 mL) and 5 M HCl/ether (9 mL) was added. The mixture was stirred at room temperature for 3 h. The precipitated hydrochloride salt was filtered off and washed thoroughly with ether. The hydrochloride was dissolved in EtOAc/MeOH/...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1C[NH]CC[NH]1
C1C[NH]CCN1
c1ccccc1.c1cnccn1.C1C[NH]CCN1
HO-
Cl.CCOCC.CCOCC.CCOC(=O)C
null
3
COCCOc1cccc(OCCOc2nccnc2N2CCN(C(=O)OC(C)(C)C)CC2)c1>Cl.CCOCC.CCOCC.CCOC(=O)C>COCCOc1cccc(OCCOc2nccnc2N2CCNCC2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0459f422d40948fabce3b5626e5172db
COc1ccc(CO)cc1.Clc1nccnc1N1CCNCC1>>COc1ccc(COc2nccnc2N2CCNCC2)cc1
ClC1=NC=CN=C1N1CCNCC1.COC1=CC=C(CO)C=C1>>COC1=CC=C(COC2=NC=CN=C2N2CCNCC2)C=C1
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][OH:8])[cH:21][cH:22]1.Cl[c:9]1[n:10][cH:11][cH:12][n:13][c:14]1[N:15]1[CH2:16][CH2:17][NH:18][CH2:19][CH2:20]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][O:8][c:9]2[n:10][cH:11][cH:12][n:13][c:14]2[N:15]2[CH2:16][CH2:17][NH:18][CH2:19][CH2:20]2)[cH:21][cH:22]1
COc1ccc(CO)cc1.Clc1nccnc1N1CCNCC1
COc1ccc(COc2nccnc2N2CCNCC2)cc1
null
null
null
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8088ac3623a2ee47f375f73ca665bec9cf80b1384463e6e2f03125aecbcea517
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1ccc(COc2nccnc2N2CCNCC2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[#7;a:5]:[c:6]:1-[#7:7].[OH;D1;+0:8]-[C:9]-[c:10]>>[#7:7]-[c:6]1:[#7;a:5]:[c:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1]:1-[O;H0;D2;+0:8]-[C:9]-[c:10]
72
[{"value": 72.0, "product": "COC1=CC=C(COC2=NC=CN=C2N2CCNCC2)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
The title compound was prepared according to the procedure of Example 90, Step 2, starting from 2-chloro-3-(1-piperazinyl)pyrazine (0.80 g, 4.0 mmol; from Example 90, Step 1) and 4-methoxybenzyl alcohol (0.88 g, 6.4 mmol). Oil; yield 72%. MS m/z 301 (M+H)+. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cnccn1
c1cnccn1
c1ccccc1.c1cnccn1.C1C[NH]CCN1
HCl
null
null
null
COc1ccc(CO)cc1.Clc1nccnc1N1CCNCC1>>COc1ccc(COc2nccnc2N2CCNCC2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fe6be616f9574daeb2b80cc5ee418c40
Clc1cc(Cl)nc(Cl)n1.FC(F)c1nc2ccccc2[nH]1>>FC(F)c1nc2ccccc2n1-c1nc(Cl)cc(Cl)n1
O.[H-].[Na+].FC(C=1NC2=C(N1)C=CC=C2)F.ClC1=NC(=CC(=N1)Cl)Cl>>ClC1=NC(=NC(=C1)Cl)N1C(=NC2=C1C=CC=C2)C(F)F
Cl[c:13]1[n:14][c:15]([Cl:16])[cH:17][c:18]([Cl:19])[n:20]1.[F:1][CH:2]([F:3])[c:4]1[n:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]2[nH:12]1>>[F:1][CH:2]([F:3])[c:4]1[n:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]2[n:12]1-[c:13]1[n:14][c:15]([Cl:16])[cH:17][c:18]([Cl:19])[n:20]1
Clc1cc(Cl)nc(Cl)n1.FC(F)c1nc2ccccc2[nH]1
FC(F)c1nc2ccccc2n1-c1nc(Cl)cc(Cl)n1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
4298ad87b3fff687c9179de37beeb6526c6797b156d79bab2f6a2c088e12b01a
e3660767655c50df0f92afc78c794dd2af7cf646bf1430960eafd30c23bf3fa7
c1cnc(-n2cnc3ccccc32)nc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[C:6]-[c:7]1:[#7;a:8]:[c:9](:[c:10]):[c:11](:[c:12]):[nH;D2;+0:13]:1>>[C:6]-[c:7]1:[#7;a:8]:[c:9](:[c:10]):[c:11](:[c:12]):[n;H0;D3;+0:13]:1-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5]
62.2
[{"value": 62.0, "product": "ClC1=NC(=NC(=C1)Cl)N1C(=NC2=C1C=CC=C2)C(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.2, "product": "ClC1=NC(=NC(=C1)Cl)N1C(=NC2=C1C=CC=C2)C(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
0.84 g (5 mmol) of 2-difluoromethylbenzimidazole dissolved in DMF (25 ml) was added and reacted with 60% sodium hydride (0.24 g, 6 mmol) at room temperature for 30 minutes. This suspension was added to a solution of 2,4,6-trichloropyrimidine (0.92 g, 5 mmol) dissolved in DMF (25 ml) and stirred at room temperature for ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1cncnc1.c1ccc2[nH]cnc2c1
c1nc2ccccc2[nH]1.c1cncnc1
c1nc2ccccc2[nH]1.c1cncnc1
HCl
CN(C)C=O
null
1.5
Clc1cc(Cl)nc(Cl)n1.FC(F)c1nc2ccccc2[nH]1>CN(C)C=O>FC(F)c1nc2ccccc2n1-c1nc(Cl)cc(Cl)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1024bf11d77148c69155ab9d4a3af94c
C1COCCN1.C[C@@H]1OCCN(c2cc(Cl)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C>>C[C@@H]1OCCN(c2cc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
ClC1=NC(=NC(=C1)N1[C@@H]([C@@H](OCC1)C)C)N1C(=NC2=C1C=CC=C2)C(F)F.N1CCOCC1>>FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC=C2)F
[NH:10]1[CH2:11][CH2:12][O:13][CH2:14][CH2:15]1.Cl[c:9]1[cH:8][c:7]([N:6]2[CH2:5][CH2:4][O:3][C@@H:2]([CH3:1])[C@H:31]2[CH3:32])[n:30][c:17](-[n:18]2[c:19]([CH:20]([F:21])[F:22])[n:23][c:24]3[cH:25][cH:26][cH:27][cH:28][c:29]23)[n:16]1>>[CH3:1][C@@H:2]1[O:3][CH2:4][CH2:5][N:6]([c:7]2[cH:8][c:9]([N:10]3[CH2:11][CH2:12][...
C1COCCN1.C[C@@H]1OCCN(c2cc(Cl)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
C[C@@H]1OCCN(c2cc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
null
null
null
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
b6ba2533a469a91b7ece94b4a523fa9d9d9bc584236787b5a2be96cdf7a917fc
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[#7;a:4]):[#7;a:5]:[c:6](-[#7:7]):[c:8]:1.[#8:9]1-[C:10]-[C:11]-[NH;D2;+0:12]-[C:13]-[C:14]-1>>[#7:7]-[c:6]1:[#7;a:5]:[c:3](-[#7;a:4]):[#7;a:2]:[c;H0;D3;+0:1](-[N;H0;D3;+0:12]2-[C:11]-[C:10]-[#8:9]-[C:14]-[C:13]-2):[c:8]:1
91.7
[{"value": 90.0, "product": "FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC=C2)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 91.7, "product": "FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC=C2)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
1
HOUR
0.84 g (5 mmol) of 2-difluoromethylbenzimidazole dissolved in DMF (25 ml) was added and reacted with 60% sodium hydride (0.24 g, 6 mmol) at room temperature for 30 minutes. This suspension was added to a solution of 2,4,6-trichloropyrimidine (0.92 g, 5 mmol) dissolved in DMF (25 ml) and stirred at room temperature for ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1COCCN1.c1cncnc1
c1cncnc1.C1COCC[NH]1
C1COCC[NH]1.c1cncnc1.C1COCC[NH]1.c1nc2ccccc2[nH]1
HCl
null
70
1
C1COCCN1.C[C@@H]1OCCN(c2cc(Cl)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C>>C[C@@H]1OCCN(c2cc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-41380e62366441e898e069d6f8e656f9
Clc1nc(Cl)nc(N2CCOCC2)n1.FC(F)c1nc2ccccc2[nH]1>>FC(F)c1nc2ccccc2n1-c1nc(Cl)nc(N2CCOCC2)n1
ClC1=NC(=NC(=N1)Cl)N1CCOCC1.FC(C=1NC2=C(N1)C=CC=C2)F.C([O-])([O-])=O.[K+].[K+].CN(C)C=O>>ClC1=NC(=NC(=N1)N1CCOCC1)N1C(=NC2=C1C=CC=C2)C(F)F
Cl[c:13]1[n:14][c:15]([Cl:16])[n:17][c:18]([N:19]2[CH2:20][CH2:21][O:22][CH2:23][CH2:24]2)[n:25]1.[F:1][CH:2]([F:3])[c:4]1[n:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]2[nH:12]1>>[F:1][CH:2]([F:3])[c:4]1[n:5][c:6]2[cH:7][cH:8][cH:9][cH:10][c:11]2[n:12]1-[c:13]1[n:14][c:15]([Cl:16])[n:17][c:18]([N:19]2[CH2:20][CH2:21][O:22]...
Clc1nc(Cl)nc(N2CCOCC2)n1.FC(F)c1nc2ccccc2[nH]1
FC(F)c1nc2ccccc2n1-c1nc(Cl)nc(N2CCOCC2)n1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
de8ca90b6a87d8cb2c34d2d3043201922cff5cf5653513773b5948279865a7ce
e3660767655c50df0f92afc78c794dd2af7cf646bf1430960eafd30c23bf3fa7
c1ccc2c(c1)ncn2-c1ncnc(N2CCOCC2)n1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[#7:6]):[#7;a:7]:1.[C:8]-[c:9]1:[#7;a:10]:[c:11](:[c:12]):[c:13](:[c:14]):[nH;D2;+0:15]:1>>[#7:6]-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[n;H0;D3;+0:15]2:[c:13](:[c:14]):[c:11](:[c:12]):[#7;a:10]:[c:9]:2-[C:8]):[#7;a:7]:1
86
[{"value": 86.0, "product": "ClC1=NC(=NC(=N1)N1CCOCC1)N1C(=NC2=C1C=CC=C2)C(F)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 85.6, "product": "ClC1=NC(=NC(=N1)N1CCOCC1)N1C(=NC2=C1C=CC=C2)C(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
11.8 g (50 mmol) of 2,4-dichloro-6-morpholino-1,3,5-triazine, 8.41 g (50 mmol) of 2-difluoromethyl-benzimidazole and 55.3 g (400 mmol) of anhydrous potassium carbonate added to DMF (250 ml) were stirred at room temperature for 16 hours. The reaction solution was poured into water and the resulting precipitates were was...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ncncn1.c1ccc2[nH]cnc2c1
c1nc2ccccc2[nH]1.c1ncncn1
c1nc2ccccc2[nH]1.c1ncncn1.C1COCC[NH]1
HCl
O
null
16
Clc1nc(Cl)nc(N2CCOCC2)n1.FC(F)c1nc2ccccc2[nH]1>O>FC(F)c1nc2ccccc2n1-c1nc(Cl)nc(N2CCOCC2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ce4b2890a50f4b1cb2d14522ba431039
C[C@@H]1NCCO[C@@H]1C.FC(F)c1nc2ccccc2n1-c1nc(Cl)nc(N2CCOCC2)n1>>C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
ClC1=NC(=NC(=N1)N1CCOCC1)N1C(=NC2=C1C=CC=C2)C(F)F.Cl.C[C@@H]1[C@@H](NCCO1)C.C([O-])([O-])=O.[K+].[K+].CN(C)C=O>>FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC=C2)F
[CH3:1][C@H:2]1[O:3][CH2:4][CH2:5][NH:6][C@H:31]1[CH3:32].Cl[c:7]1[n:8][c:9]([N:10]2[CH2:11][CH2:12][O:13][CH2:14][CH2:15]2)[n:16][c:17](-[n:18]2[c:19]([CH:20]([F:21])[F:22])[n:23][c:24]3[cH:25][cH:26][cH:27][cH:28][c:29]23)[n:30]1>>[CH3:1][C@@H:2]1[O:3][CH2:4][CH2:5][N:6]([c:7]2[n:8][c:9]([N:10]3[CH2:11][CH2:12][O:13]...
C[C@@H]1NCCO[C@@H]1C.FC(F)c1nc2ccccc2n1-c1nc(Cl)nc(N2CCOCC2)n1
C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
null
null
O
Heteroatom Alkylation and Arylation
Ullmann-Goldberg Substitution amine
93a150f14ca1246791130f1830975e6ad6685a37209989974b5c61095e16cfc0
b6b8e2cdb45054a35f5e8157d624f852c0601a09401556706e166b19536eb7a7
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3](-[#7;a:4]):[#7;a:5]:[c:6]:[#7;a:7]:1.[C;D1;H3:8]-[C:9]1-[C:10]-[#8:11]-[C:12]-[C:13]-[NH;D2;+0:14]-1>>[#7;a:4]-[c:3]1:[#7;a:5]:[c:6]:[#7;a:7]:[c;H0;D3;+0:1](-[N;H0;D3;+0:14]2-[C:13]-[C:12]-[#8:11]-[C:10]-[C:9]-2-[C;D1;H3:8]):[#7;a:2]:1
87
[{"value": 87.0, "product": "FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC=C2)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.0, "product": "FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC=C2)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
11.8 g (50 mmol) of 2,4-dichloro-6-morpholino-1,3,5-triazine, 8.41 g (50 mmol) of 2-difluoromethyl-benzimidazole and 55.3 g (400 mmol) of anhydrous potassium carbonate added to DMF (250 ml) were stirred at room temperature for 16 hours. The reaction solution was poured into water and the resulting precipitates were was...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Secondary amine
Tertiary amine
C1COCCN1.c1ncncn1
C1COCC[NH]1.c1ncncn1
C1COCC[NH]1.c1ncncn1.C1COCC[NH]1.c1nc2ccccc2[nH]1
HCl
O
null
16
C[C@@H]1NCCO[C@@H]1C.FC(F)c1nc2ccccc2n1-c1nc(Cl)nc(N2CCOCC2)n1>O>C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)[C@@H]1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-973a0255d7144497b4821cb1ab64dd54
FC(F)c1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCSCC2)n1>>O=S1CCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)CC1
FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCSCC1)C=CC=C2)F.ClC1=CC(=CC=C1)C(=O)OO.O>>FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCS(CC1)=O)C=CC=C2)F
[S:2]1[CH2:3][CH2:4][N:5]([c:6]2[n:7][c:8]([N:9]3[CH2:10][CH2:11][O:12][CH2:13][CH2:14]3)[n:15][c:16](-[n:17]3[c:18]([CH:19]([F:20])[F:21])[n:22][c:23]4[cH:24][cH:25][cH:26][cH:27][c:28]34)[n:29]2)[CH2:30][CH2:31]1>>[O:1]=[S:2]1[CH2:3][CH2:4][N:5]([c:6]2[n:7][c:8]([N:9]3[CH2:10][CH2:11][O:12][CH2:13][CH2:14]3)[n:15][c:...
FC(F)c1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCSCC2)n1
O=S1CCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)CC1
null
null
ClCCl
Oxidation
Sulfanyl to sulfinyl
c85a23881a8c3a3231ed34b602ece3d962b8a98fadea32e6ade07ff31a14194b
f5f6bb6ca76a2267cd589767b4d67e7a17ab1ac383eeb6143dcd5d92e00e1b6a
O=S1CCN(c2nc(N3CCOCC3)nc(-n3cnc4ccccc43)n2)CC1
[#7:1]1-[C:2]-[C:3]-[S;H0;D2;+0:4]-[C:5]-[C:6]-1>>[O;D1;H0:7]=[S;H0;D3;+0:4]1-[C:3]-[C:2]-[#7:1]-[C:6]-[C:5]-1
42.9
[{"value": 42.0, "product": "FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCS(CC1)=O)C=CC=C2)F", "details": "PERCENTYIELD", "is_desired": false}, {"value": 42.9, "product": "FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCS(CC1)=O)C=CC=C2)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
0.61 g (1.4 mmol) of 2-(2-difluoromethylbenzimidazol-1-yl)-4-morpholino-6-thiomorpholino-1,3,5-triazine dissolved in dichloromethane (20 ml) was added with m-chloroperbenzoic acid (0.35 g, 2.0 mmol) and stirred at room temperature for 16 hours. The reaction solution was poured into water and extracted with ethyl acetat...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Sulfoxide
C1CSCC[NH]1
C1CSCC[NH]1
C1CSCC[NH]1.c1ncncn1.C1COCC[NH]1.c1nc2ccccc2[nH]1
null
ClCCl
null
16
FC(F)c1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCSCC2)n1>ClCCl>O=S1CCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4ccccc43)n2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ea4fa84f58b14006b5a9e9d83c326429
Clc1nc(N2CCOCC2)nc(N2CCOCC2)n1.Nc1nc2ccccc2[nH]1>>Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
O.[H-].[Na+].NC=1NC2=C(N1)C=CC=C2.ClC1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1>>NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2
Cl[c:11]1[n:12][c:13]([N:14]2[CH2:15][CH2:16][O:17][CH2:18][CH2:19]2)[n:20][c:21]([N:22]2[CH2:23][CH2:24][O:25][CH2:26][CH2:27]2)[n:28]1.[NH2:1][c:2]1[n:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[nH:10]1>>[NH2:1][c:2]1[n:3][c:4]2[cH:5][cH:6][cH:7][cH:8][c:9]2[n:10]1-[c:11]1[n:12][c:13]([N:14]2[CH2:15][CH2:16][O:17][CH2:18]...
Clc1nc(N2CCOCC2)nc(N2CCOCC2)n1.Nc1nc2ccccc2[nH]1
Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
de8ca90b6a87d8cb2c34d2d3043201922cff5cf5653513773b5948279865a7ce
e3660767655c50df0f92afc78c794dd2af7cf646bf1430960eafd30c23bf3fa7
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[#7:6]):[#7;a:7]:1.[N;D1;H2:8]-[c:9]1:[#7;a:10]:[c:11](:[c:12]):[c:13](:[c:14]):[nH;D2;+0:15]:1>>[#7:6]-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[n;H0;D3;+0:15]2:[c:9](-[N;D1;H2:8]):[#7;a:10]:[c:11](:[c:12]):[c:13]:2:[c:14]):[#7;a:7]:1
93
[{"value": 93.0, "product": "NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.6, "product": "NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
9.32 g (70 mmol) of 2-aminobenzimidazole dissolved in DMF (300 ml) was added and reacted with 60% sodium hydride (2.80 g, 70 mmol) at room temperature for 30 minutes. This suspension was added to a solution of 14.3 g (50 mmol) of 2-chloro-4,6-dimorpholino-1,3,5-triazine dissolved in DMF (200 ml) and stirred at room tem...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
null
c1ncncn1.c1ccc2[nH]cnc2c1
c1nc2ccccc2[nH]1.c1ncncn1
c1nc2ccccc2[nH]1.c1ncncn1.C1COCC[NH]1.C1COCC[NH]1
HCl
CN(C)C=O
null
2
Clc1nc(N2CCOCC2)nc(N2CCOCC2)n1.Nc1nc2ccccc2[nH]1>CN(C)C=O>Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8d5cb1d72fbf4e4bb26686f07a0a19c8
CC(=O)O.Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1>>CC(=O)Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
C(Cl)(Cl)Cl.NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2.C(C)(=O)O.C1CCC(CC1)N=C=NC2CCCCC2>>C(C)(=O)NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2
O[C:2]([CH3:1])=[O:3].[NH2:4][c:5]1[n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[n:13]1-[c:14]1[n:15][c:16]([N:17]2[CH2:18][CH2:19][O:20][CH2:21][CH2:22]2)[n:23][c:24]([N:25]2[CH2:26][CH2:27][O:28][CH2:29][CH2:30]2)[n:31]1>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[n:6][c:7]2[cH:8][cH:9][cH:10][cH:11][c:12]2[n:13]1-[c:14]1[n:15]...
CC(=O)O.Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
CC(=O)Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
null
null
O
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[#7;a:4]:[c:5](-[#7;a:6]1:[c:7]:[c:8]:[#7;a:9]:[c:10]:1-[NH2;D1;+0:11]):[#7;a:12]>>[#7;a:4]:[c:5](-[#7;a:6]1:[c:7]:[c:8]:[#7;a:9]:[c:10]:1-[NH;D2;+0:11]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3]):[#7;a:12]
73
[{"value": 73.0, "product": "C(C)(=O)NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.0, "product": "C(C)(=O)NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
9.32 g (70 mmol) of 2-aminobenzimidazole dissolved in DMF (300 ml) was added and reacted with 60% sodium hydride (2.80 g, 70 mmol) at room temperature for 30 minutes. This suspension was added to a solution of 14.3 g (50 mmol) of 2-chloro-4,6-dimorpholino-1,3,5-triazine dissolved in DMF (200 ml) and stirred at room tem...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1nc2ccccc2[nH]1.c1ncncn1.C1COCC[NH]1.C1COCC[NH]1
HO-
O
null
4
CC(=O)O.Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1>O>CC(=O)Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eac1321f2c99465f8fa75f66bfd88b15
Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1.O=COCCl>>COC(=O)Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
CN(C)C=O.NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2.[H-].[Na+].ClCOC=O>>COC(=O)NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2
[NH2:5][c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[n:14]1-[c:15]1[n:16][c:17]([N:18]2[CH2:19][CH2:20][O:21][CH2:22][CH2:23]2)[n:24][c:25]([N:26]2[CH2:27][CH2:28][O:29][CH2:30][CH2:31]2)[n:32]1.Cl[CH2:1][O:2][CH:3]=[O:4]>>[CH3:1][O:2][C:3](=[O:4])[NH:5][c:6]1[n:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[n:14]1-[...
Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1.O=COCCl
COC(=O)Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
null
null
O
Protection
OtherReaction
818a2638852ca067e1660d3f7cba4ccd667da7676c6594aef25d50435f6412db
d511adec1b387885496ae9a429ba76ae4c5fd3f4cd4823260b0f617a8bf4476d
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
Cl-[CH2;D2;+0:1]-[#8:2]-[CH;D2;+0:3]=[O;D1;H0:4].[#7;a:5]:[c:6](-[#7;a:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:1-[NH2;D1;+0:12]):[#7;a:13]>>[#7;a:5]:[c:6](-[#7;a:7]1:[c:8]:[c:9]:[#7;a:10]:[c:11]:1-[NH;D2;+0:12]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[#8:2]-[CH3;D1;+0:1]):[#7;a:13]
46
[{"value": 46.0, "product": "COC(=O)NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 45.4, "product": "COC(=O)NC1=NC2=C(N1C1=NC(=NC(=N1)N1CCOCC1)N1CCOCC1)C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
0.19 g (0.50 mmol) of 2-(2-aminobenzimidazol-1-yl)-4,6-dimorpholino-1,3,5-triazine synthesized in (1) of the Example 6 and 60% sodium hydride (24 mg, 0.60 mmol) added to DMF (2 ml) were reacted at room temperature for 1 hour. The reaction mixture was added and reacted with 0.040 ml (0.55 mmol) of chloromethylformate at...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Primary amine
Carbamic ester.Ether
null
null
c1nc2ccccc2[nH]1.c1ncncn1.C1COCC[NH]1.C1COCC[NH]1
HCl
O
null
null
Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1.O=COCCl>O>COC(=O)Nc1nc2ccccc2n1-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ded3e55de6ba4c58b7ab83aa957d0d54
O=[N+]([O-])c1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1.O=[N+]([O-])c1ccc2nc(C(F)F)n(-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)c2c1>>Nc1ccc2nc(C(F)F)n(-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)c2c1
FC(C=1NC2=C(N1)C=CC=C2)F.FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1CCOCC1)N1CCOCC1)C=CC(=C2)[N+](=O)[O-])F.FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1CCOCC1)N1CCOCC1)C=C(C=C2)[N+](=O)[O-])F>>NC=1C=CC2=C(N(C(=N2)C(F)F)C2=NC(=CC(=N2)N2CCOCC2)N2CCOCC2)C1
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][c:5]2[n:6](-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)[c:7]([CH:8]([F:9])[F:10])[n:11][c:30]2[cH:31]1.O=[N+]([O-])c1ccc2nc(C(F)F)n(-[c:12]3[n:13][c:14]([N:15]4[CH2:16][CH2:17][O:18][CH2:19][CH2:20]4)[cH:21][c:22]([N:23]4[CH2:24][CH2:25][O:26][CH2:27][CH2:28]4)[n:29]3)c2c1>>[NH2:1][c:2]1[cH:3][cH:4][...
O=[N+]([O-])c1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1.O=[N+]([O-])c1ccc2nc(C(F)F)n(-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)c2c1
Nc1ccc2nc(C(F)F)n(-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)c2c1
null
null
null
Functional Group Interconversion
OtherReaction
4792b62a0e5fb6412b5601e7af951cb5e624b3e84008e1c31e06298263fdca44
4c2e6555ce5dfeed8f764b785e50f9149644539fa987a33281a90ed9b866b296
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
F-C(-F)-c1:n:c2:c:c:c(-[N+](=O)-[O-]):c:c:2:n:1-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].O=[N+;H0;D3:6](-[O-])-[c:7]1:[c:8]:[c:9]2:[n;H0;D2;+0:10]:[c:11](-[C:12]):[n;H0;D3;+0:13](-c3:n:c(-N4-C-C-O-C-C-4):c:c(-N4-C-C-O-C-C-4):n:3):[c:14]:2:[c:15]:[c:16]:1>>[C:12]-[c:11]1:[n;H0;D2;+0:13]:[c:14]2:[c:15]:[c:16]:[c:7]...
88
[{"value": 88.0, "product": "NC=1C=CC2=C(N(C(=N2)C(F)F)C2=NC(=CC(=N2)N2CCOCC2)N2CCOCC2)C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
In accordance with the procedure of the Example 1 except that 2-difluoromethylbenzimidazole in (1) of the Example 1 was replaced by 2-difluoro-6-nitrobenzimidazole, a mixture of 2-(2-difluoromethyl-5-nitrobenzimidazol-1-yl)-4,6-dimorpholinopyrimidine with 2-(2-difluoromethyl-6-nitrobenzimidazol-1-yl)-4,6-dimorpholinopy...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Secondary halide.Ether.Ether.Nitro group.Nitro group.Tertiary amine.Tertiary amine
Primary amine
c1cncnc1.C1COCCN1.C1COCCN1.c1ccc2[nH]cnc2c1.c1ccc2[nH]cnc2c1.c1cncnc1
c1ccc2[nH]cnc2c1.c1cncnc1
c1ccc2[nH]cnc2c1.c1cncnc1.C1COCC[NH]1.C1COCC[NH]1
HF
null
null
null
O=[N+]([O-])c1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1.O=[N+]([O-])c1ccc2nc(C(F)F)n(-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)c2c1>>Nc1ccc2nc(C(F)F)n(-c3nc(N4CCOCC4)cc(N4CCOCC4)n3)c2c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d9ba8b48dcf744dfb37d5d925a99469d
C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4cc(O[Si](C)(C)C(C)(C)C)ccc43)n2)[C@@H]1C>>C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4cc(O)ccc43)n2)[C@@H]1C
[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.FC(C=1NC2=C(N1)C=CC=C2)F.FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC(=C2)O[Si](C)(C)C(C)(C)C)F.FC(C=1NC2=C(N1)C(=C(C(=C2O[SiH3])C(C)(C)C)C)C)F>>FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC(=C2)O)F
CC(C)(C)[Si](C)(C)[O:27][c:26]1[cH:25][c:24]2[n:23][c:19]([CH:20]([F:21])[F:22])[n:18](-[c:17]3[n:16][c:9]([N:10]4[CH2:11][CH2:12][O:13][CH2:14][CH2:15]4)[n:8][c:7]([N:6]4[CH2:5][CH2:4][O:3][C@@H:2]([CH3:1])[C@H:32]4[CH3:33])[n:31]3)[c:30]2[cH:29][cH:28]1>>[CH3:1][C@@H:2]1[O:3][CH2:4][CH2:5][N:6]([c:7]2[n:8][c:9]([N:10...
C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4cc(O[Si](C)(C)C(C)(C)C)ccc43)n2)[C@@H]1C
C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4cc(O)ccc43)n2)[C@@H]1C
null
null
O.C1CCOC1
Deprotection
Alcohol deprotection from silyl ethers
e70131badc7d7d580ed75b2dfb3ce6df2a5f496b2119611cf5354e1267babe73
b09ece7bccc3ff762f4ff5407ad846fffba6d6a63735853c86a86d29904f54ed
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)nc(N2CCOCC2)n1
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]:[c:5]:[#7;a:6]>>[#7;a:6]:[c:5]:[c:4]:[c:2](-[OH;D1;+0:1]):[c:3]
79
[{"value": 79.0, "product": "FC(C1=NC2=C(N1C1=NC(=NC(=N1)N1[C@@H]([C@@H](OCC1)C)C)N1CCOCC1)C=CC(=C2)O)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
In accordance with the procedure of the Example 4 except that 2-difluoromethylbenzimidazole in (1) of the Example 4 was replaced by 2-difluoromethyl-5-tert-butyldimethyl-silyloxybenzimidazole, obtained was 2-(2-difluoromethyl-5-tert-butyldimethylsilyloxybenzimidazol-1-yl)-4-(cis-2,3-dimethylmorpholino)-6-morpholino-1,3...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Aromatic alcohol
null
null
C1COCC[NH]1.c1ncncn1.C1COCC[NH]1.c1ccc2[nH]cnc2c1
Other
O.C1CCOC1
null
0.5
C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4cc(O[Si](C)(C)C(C)(C)C)ccc43)n2)[C@@H]1C>O.C1CCOC1>C[C@@H]1OCCN(c2nc(N3CCOCC3)nc(-n3c(C(F)F)nc4cc(O)ccc43)n2)[C@@H]1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1e6a466c51cc492e9ad3e90bd07420f0
CC(C)(C)[Si](C)(C)Oc1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1>>Oc1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.FC(C=1NC2=C(N1)C=CC=C2)F.FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1CCOCC1)N1CCOCC1)C=CC(=C2)O[Si](C)(C)C(C)(C)C)F.FC(C=1NC2=C(N1)C=CC(=C2)O[Si](C)(C)C(C)(C)C)F>>FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1CCOCC1)N1CCOCC1)C=CC(=C2)O)F
CC(C)(C)[Si](C)(C)[O:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([cH:7]1)[n:8][c:9]([CH:10]([F:11])[F:12])[n:13]2-[c:14]1[n:15][c:16]([N:17]2[CH2:18][CH2:19][O:20][CH2:21][CH2:22]2)[cH:23][c:24]([N:25]2[CH2:26][CH2:27][O:28][CH2:29][CH2:30]2)[n:31]1>>[OH:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([cH:7]1)[n:8][c:9]([CH:10]([F:11])[F:12])[n:1...
CC(C)(C)[Si](C)(C)Oc1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
Oc1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
null
null
O.C1CCOC1
Deprotection
Alcohol deprotection from silyl ethers
e70131badc7d7d580ed75b2dfb3ce6df2a5f496b2119611cf5354e1267babe73
b09ece7bccc3ff762f4ff5407ad846fffba6d6a63735853c86a86d29904f54ed
c1ccc2c(c1)ncn2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]:[c:5]:[#7;a:6]>>[#7;a:6]:[c:5]:[c:4]:[c:2](-[OH;D1;+0:1]):[c:3]
93
[{"value": 93.0, "product": "FC(C1=NC2=C(N1C1=NC(=CC(=N1)N1CCOCC1)N1CCOCC1)C=CC(=C2)O)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
In accordance with the procedure of the Example 1 except that 2-difluoromethylbenzimidazole in (1) of the Example 1 was replaced by 2-difluoromethyl-5-tert-butyldimethylsilyloxybenzimidazole, obtained was 2-(2-difluoromethyl-5-tert-butyldimethylsilyloxybenzimidazol-1-yl)-4,6-dimorpholinopyrimidine. 0.55 g (1.0 mmol) of...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Aromatic alcohol
null
null
c1ccc2nc[nH]c2c1.c1cncnc1.C1COCC[NH]1.C1COCC[NH]1
Other
O.C1CCOC1
null
0.5
CC(C)(C)[Si](C)(C)Oc1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1>O.C1CCOC1>Oc1ccc2c(c1)nc(C(F)F)n2-c1nc(N2CCOCC2)cc(N2CCOCC2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b005b6f337a44f94b9a0bf0c978e4792
Cc1cc(C)cc(-c2cc3ncnc(O)c3s2)c1.O=P(Cl)(Cl)Cl>>Cc1cc(C)cc(-c2cc3ncnc(Cl)c3s2)c1
OC=1C2=C(N=CN1)C=C(S2)C2=CC(=CC(=C2)C)C.C(C)(C)N(CC)C(C)C.P(=O)(Cl)(Cl)Cl>>ClC=1C2=C(N=CN1)C=C(S2)C2=CC(=CC(=C2)C)C
O[c:14]1[n:13][cH:12][n:11][c:10]2[cH:9][c:8](-[c:7]3[cH:6][c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:18]3)[s:17][c:16]21.O=P(Cl)(Cl)[Cl:15]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:7](-[c:8]2[cH:9][c:10]3[n:11][cH:12][n:13][c:14]([Cl:15])[c:16]3[s:17]2)[cH:18]1
Cc1cc(C)cc(-c2cc3ncnc(O)c3s2)c1.O=P(Cl)(Cl)Cl
Cc1cc(C)cc(-c2cc3ncnc(Cl)c3s2)c1
null
null
null
Functional Group Interconversion
Alcohol to chloride_POCl3_ortho
c5bd6f721b4a732e8f530df375174d18cc558944df73419315d063a44729e72f
e71580a8ffadb7b2717ecd7d68c1d3c0ca161ba5e6a787a49dad5a1359adc993
c1ccc(-c2cc3ncncc3s2)cc1
Cl-P(-Cl)(=O)-[Cl;H0;D1;+0:1].O-[c;H0;D3;+0:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]2:[c:7]:[c:8]:[#16;a:9]:[c:10]:2:1>>[Cl;H0;D1;+0:1]-[c;H0;D3;+0:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]2:[c:7]:[c:8]:[#16;a:9]:[c:10]:2:1
null
[]
100
CELSIUS
null
null
The hydroxy compound prepared in Step 1 was treated with phosphorous oxychloride (150 mL) and diisopropylethylamine (2 mL). The mixture was then heated at 100° C. for 4 hours. The solvents were evaporated under reduced pressure and the residue was carefully treated with ice water. The resulting solid was filtered off a...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
Aromatic halide
c1ncc2sccc2n1
c1ncc2sccc2n1
c1ccccc1.c1ncc2sccc2n1
HCl
null
100
null
Cc1cc(C)cc(-c2cc3ncnc(O)c3s2)c1.O=P(Cl)(Cl)Cl>>Cc1cc(C)cc(-c2cc3ncnc(Cl)c3s2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4d12ac80a56d479baf43142f1db2788d
COC(=O)CN.O=C1CCCCCC1>>O=C(O)CNC1CCCCCC1
C1(CCCCCC1)=O.COC(CN)=O>>C1(CCCCCC1)NCC(=O)O
C[O:3][C:2](=[O:1])[CH2:4][NH2:5].O=[C:6]1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1>>[O:1]=[C:2]([OH:3])[CH2:4][NH:5][CH:6]1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1
COC(=O)CN.O=C1CCCCCC1
O=C(O)CNC1CCCCCC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
7ea5121718be1ecc742f905d3734383e45859d783523b6197248271234304b8c
54e31965a8ebe7ac0cdd3327194966ab957cb5aa1af511ad8ea20929465150a5
C1CCCCCC1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[NH2;D1;+0:5].O=[C;H0;D3;+0:6](-[C:7]-[C:8])-[C:9]-[C:10]>>[C:8]-[C:7]-[CH;D3;+0:6](-[NH;D2;+0:5]-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1])-[C:9]-[C:10]
null
[]
null
null
null
null
N-Cycloheptylglycine was synthesized by reductive amination of cycloheptanone with glycine methyl ester following the procedure described in Gera et al., Immunopharmacology. 33:174–177 (1996). The crude product was converted to the N-Boc derivative (mp, 89–90° C.). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Ester.Primary amine
Carboxylic acid.Secondary amine
C1CCCCCC1
C1CCCCCC1
C1CCCCCC1
HO-
null
null
null
COC(=O)CN.O=C1CCCCCC1>>O=C(O)CNC1CCCCCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fa704ecb2dbe442f93a503e20069bbcd
O=C(O)C=Cc1ccncc1>>O=C(O)CCC1CCNCC1
N1=CC=C(C=C1)C=CC(=O)O.[H][H]>>N1CCC(CC1)CCC(=O)O
[O:1]=[C:2]([OH:3])[CH:4]=[CH:5][c:6]1[cH:7][cH:8][n:9][cH:10][cH:11]1>>[O:1]=[C:2]([OH:3])[CH2:4][CH2:5][CH:6]1[CH2:7][CH2:8][NH:9][CH2:10][CH2:11]1
O=C(O)C=Cc1ccncc1
O=C(O)CCC1CCNCC1
null
[Ru]
O.N
Reduction
OtherReaction
8a6c78a63989dd47e282eb33ae5ce6bfcead5defaa210963e9125c31297ee886
2b7f370a519e29b4dede190aa36b37f30822496e32f2c8bfa9736e631bde52e2
C1CCNCC1
[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[CH;D2;+0:4]=[CH;D2;+0:5]-[c;H0;D3;+0:6]1:[cH;D2;+0:7]:[cH;D2;+0:8]:[n;H0;D2;+0:9]:[cH;D2;+0:10]:[cH;D2;+0:11]:1>>[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[CH;D3;+0:6]1-[CH2;D2;+0:7]-[CH2;D2;+0:8]-[NH;D2;+0:9]-[CH2;D2;+0:10]-[CH2;D2;+0:11]-1
100
[{"value": 100.0, "product": "N1CCC(CC1)CCC(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 97.7, "product": "N1CCC(CC1)CCC(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 3-pyridin4-yl-acrylic acid (4.20 g, 28.0 mmol) in water (50 mL) and ammonia (aq, 25%, 4 mL) was hydrogenated at 60 bar in a high pressure steel autoclave in presence of ruthenium (5% on alumina, 439 mg). When hydrogen pressure remained constant (3 days) the catalyst was removed from the reaction mixture b...
10.6084/m9.figshare.5104873.v1
null
null
Secondary amine
c1ccncc1
C1CCNCC1
C1CCNCC1
null
[Ru].O.N
null
null
O=C(O)C=Cc1ccncc1>[Ru].O.N>O=C(O)CCC1CCNCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-503d8f8f951340d2a25790799eb1eb45
CC(C)(C)OC(=O)N1CCC(CC(CSCc2ccccc2)C(=O)O)CC1>>CC(C)(C)OC(=O)N1CCC(CC(CS)C(=O)O)CC1
[Cl-].[NH4+].[Na].C(C)(C)(C)OC(=O)N1CCC(CC1)CC(CSCC1=CC=CC=C1)C(=O)O.N>>C(C)(C)(C)OC(=O)N1CCC(CC1)CC(CS)C(=O)O
c1ccc(C[S:15][CH2:14][CH:13]([CH2:12][CH:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:20][CH2:19]2)[C:16](=[O:17])[OH:18])cc1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][CH:13]([CH2:14][SH:15])[C:16](=[O:17])[OH:18])[CH2:19][CH2:20]1
CC(C)(C)OC(=O)N1CCC(CC(CSCc2ccccc2)C(=O)O)CC1
CC(C)(C)OC(=O)N1CCC(CC(CS)C(=O)O)CC1
null
null
C1CCOC1
Deprotection
OtherReaction
8ede657ec13277980662af24e502b19505abce30b66d95f1c70163f9a07caa47
d0652a71194d478b6d145ca18f942c41b2e93fe2aec41553ada2c2882bb6a1a5
C1CCNCC1
[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[C:4]-[C:5]-[S;H0;D2;+0:6]-C-c1:c:c:c:c:c:1>>[O;D1;H0:1]=[C:2](-[O;D1;H1:3])-[C:4]-[C:5]-[SH;D1;+0:6]
100.7
[{"value": 100.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CC(CS)C(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 100.7, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CC(CS)C(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Sodium metal (513 mg, 22.5 mmol) was added in portions during 5 min. to a solution of 4-(3-Benzylsulfanyl-2-carboxy-propyl)-piperidine-1-carboxylic acid tert-butyl ester (0.9 g, 2.29 mmol) in THF (45 mL) and liquid ammonia (50 mL) at −60° C. under argon. After stirring for 15 min. ammonium chloride (1.7 g, 31.5 mmol) w...
10.6084/m9.figshare.5104873.v1
null
Monosulfide
Aliphatic thiol
c1ccccc1
null
C1CC[NH]CC1
Other
C1CCOC1
null
null
CC(C)(C)OC(=O)N1CCC(CC(CSCc2ccccc2)C(=O)O)CC1>C1CCOC1>CC(C)(C)OC(=O)N1CCC(CC(CS)C(=O)O)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-65be9be147ec4d6cba76109aff30097f
O=C(O)C(CS)CC1CCNCC1.O=C(O)C(F)(F)F>>CC(=O)N1CCC(CC(CS)C(=O)O)CC1
OC(=O)C(F)(F)F.SCC(C(=O)O)CC1CCNCC1>>C(C)(=O)N1CCC(CC1)CC(C(=O)O)CS
[NH:4]1[CH2:5][CH2:6][CH:7]([CH2:8][CH:9]([CH2:10][SH:11])[C:12](=[O:13])[OH:14])[CH2:15][CH2:16]1.O[C:2]([C:1](F)(F)F)=[O:3]>>[CH3:1][C:2](=[O:3])[N:4]1[CH2:5][CH2:6][CH:7]([CH2:8][CH:9]([CH2:10][SH:11])[C:12](=[O:13])[OH:14])[CH2:15][CH2:16]1
O=C(O)C(CS)CC1CCNCC1.O=C(O)C(F)(F)F
CC(=O)N1CCC(CC(CS)C(=O)O)CC1
null
null
C(C)(=O)OC(C)=O
Acylation
OtherReaction
4e665ada278c24eacee09f9a3c04c28279e21a3099f8c777c866698d929a6b64
a253cb3278e717ca1fbd16abc111e74dcfbf11461b2eecdac44191f9b4019e83
C1CCNCC1
F-[C;H0;D4;+0:1](-F)(-F)-[C;H0;D3;+0:2](-O)=[O;D1;H0:3].[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[C;H0;D3;+0:2](-[CH3;D1;+0:1])=[O;D1;H0:3])-[C:7]-[C:8]
80.2
[{"value": 80.0, "product": "C(C)(=O)N1CCC(CC1)CC(C(=O)O)CS", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.2, "product": "C(C)(=O)N1CCC(CC1)CC(C(=O)O)CS", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 2-Mercaptomethyl-3-piperidin-4-yl-propionic acid TFA salt (0.1 g, 0.32 mmol) in acetic anhydride (2 mL) was stirred over night under argon and then concentrated under reduced pressure. Purification by HPLC (10→50% acetonitrile, 0.1% TFA in water) gave the title compound (63 mg, 80%). Conditions: See react...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Carboxylic acid.Secondary amine
Tertiary amide
C1CCNCC1
C1CC[NH]CC1
C1CC[NH]CC1
Other
C(C)(=O)OC(C)=O
null
null
O=C(O)C(CS)CC1CCNCC1.O=C(O)C(F)(F)F>C(C)(=O)OC(C)=O>CC(=O)N1CCC(CC(CS)C(=O)O)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0c62e6cebadc470dbabcf15e2d3a6fe2
BrC(Br)(Br)Br.CC(C)(C)OC(=O)N1CCC(CO)CC1>>CC(C)(C)OC(=O)N1CCC(CBr)CC1
C(C)(C)(C)OC(=O)N1CCC(CC1)CO.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(Br)(Br)(Br)Br>>C(C)(C)(C)OC(=O)N1CCC(CC1)CBr
BrC(Br)(Br)[Br:13].O[CH2:12][CH:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:15][CH2:14]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][Br:13])[CH2:14][CH2:15]1
BrC(Br)(Br)Br.CC(C)(C)OC(=O)N1CCC(CO)CC1
CC(C)(C)OC(=O)N1CCC(CBr)CC1
null
null
C(C)OCC
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
C1CCNCC1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3](-[C:4])-[C:5]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](-[C:4])-[C:5]
73.1
[{"value": 73.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CBr", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.1, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CBr", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
To a solution 4-hydroxymethyl-piperidine-1-carboxylic acid tert-butyl ester (8.75 g, 40.64 mmol) in diethyl ether (200 mL) at 0° C. under nitrogen. were added triphenyl phosphine (21.32 g, 81.28 mmol) and carbon tetrabromide (26.96 g, 81.28 mmol). The mixture was allowed to warm to room temperature and stirred under ni...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
C1CC[NH]CC1
HBr
C(C)OCC
null
48
BrC(Br)(Br)Br.CC(C)(C)OC(=O)N1CCC(CO)CC1>C(C)OCC>CC(C)(C)OC(=O)N1CCC(CBr)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3766d5d750f448b4a39ea86404d088d3
CC(C)(C)OC(=O)N1CCC(CBr)CC1.CCOP(=O)(CC(=O)OC(C)(C)C)OCC.O>>CCOP(=O)(CC(=O)OC(C)(C)C)OCC.CCOP(=O)(OCC)C(CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OC(C)(C)C
C(C)(C)(C)OC(=O)N1CCC(CC1)CBr.C(C)OP(=O)(OCC)CC(=O)OC(C)(C)C.[H-].[Na+].O>>C(C)(C)(C)OC(=O)N1CCC(CC1)CC(P(=O)(OCC)OCC)C(=O)OC(C)(C)C.C(C)OP(=O)(OCC)CC(=O)OC(C)(C)C
Br[CH2:26][CH:27]1[CH2:28][CH2:29][N:30]([C:31](=[O:32])[O:33][C:34]([CH3:25])([CH3:35])[CH3:37])[CH2:38][CH2:39]1.[CH3:1][CH2:2][O:3][P:4](=[O:5])([CH2:6][C:7](=[O:8])[O:9][C:10]([CH3:11])([CH3:18])[CH3:24])[O:14][CH2:15][CH3:16].[OH2:41]>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([CH2:6][C:7](=[O:8])[O:9][C:10]([CH3:11])([CH3...
CC(C)(C)OC(=O)N1CCC(CBr)CC1.CCOP(=O)(CC(=O)OC(C)(C)C)OCC.O
CCOP(=O)(CC(=O)OC(C)(C)C)OCC.CCOP(=O)(OCC)C(CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OC(C)(C)C
null
null
CN(C)C=O
Acylation
OtherReaction
a3202466c5051a4246443792e706fa69b83b341c168f44c95f8bcecc2c14df33
8c255a91e9b3cc01ee961564874897d7dcff087be6435234c9cc2ffd1a71bc7f
C1CCNCC1
Br-[CH2;D2;+0:1]-[C:2]1-[C:3]-[C:4]-[#7:5](-[C:6](=[O;D1;H0:7])-[#8:8]-[C;H0;D4;+0:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[CH3;D1;+0:12])-[C:13]-[C:14]-1.[C:15]-[C:16](=[O;D1;H0:17])-[#8:18]-[C;H0;D4;+0:19](-[C;D1;H3:20])(-[CH3;D1;+0:21])-[CH3;D1;+0:22].[OH2;D0;+0:23]>>[#8:24]-[C:25](=[O;H0;D1;+0:23])-[CH;D3;+0:12](-[CH2;D2;...
null
[]
0
CELSIUS
0.5
HOUR
tert-Butyl diethylphosphonoacetate (75.0 g, 297.32 mmol) was added dropwise to a suspension of sodium hydride (8.03 g, 334.58 mmol) in DMF (450 mL) at 0° C. under nitrogen. The mixture was stirred at 0° C. for 0.5 h and at room temperature for 0.5 h. 4-bromomethyl-piperidine-1-carboxylic acid tert-butyl ester (20.68 g,...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ether.Boc.Boc
Ester.Ester.Ether.Boc.Boc.Boc
null
null
C1CC[NH]CC1
Br-
CN(C)C=O
0
0.5
CC(C)(C)OC(=O)N1CCC(CBr)CC1.CCOP(=O)(CC(=O)OC(C)(C)C)OCC.O>CN(C)C=O>CCOP(=O)(CC(=O)OC(C)(C)C)OCC.CCOP(=O)(OCC)C(CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c358a21ea0d542caa5807df5d9aaba60
CC(C)CC=C(CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OC(C)(C)C.COc1ccc(CS)cc1>>COc1ccc(CSC(CC(C)C)C(CC2CCN(C(=O)OC(C)(C)C)CC2)C(=O)OC(C)(C)C)cc1
O.C(C)(C)(C)OC(=O)N1CCC(CC1)CC(=CCC(C)C)C(=O)OC(C)(C)C.C([O-])([O-])=O.[K+].[K+].COC1=CC=C(C=C1)CS>>C(C)(C)(C)OC(=O)N1CCC(CC1)CC(C(CC(C)C)SCC1=CC=C(C=C1)OC)C(=O)OC(C)(C)C
[CH:9]([CH2:10][CH:11]([CH3:12])[CH3:13])=[C:14]([CH2:15][CH:16]1[CH2:17][CH2:18][N:19]([C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[CH2:27][CH2:28]1)[C:29](=[O:30])[O:31][C:32]([CH3:33])([CH3:34])[CH3:35].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][SH:8])[cH:36][cH:37]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]...
CC(C)CC=C(CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OC(C)(C)C.COc1ccc(CS)cc1
COc1ccc(CSC(CC(C)C)C(CC2CCN(C(=O)OC(C)(C)C)CC2)C(=O)OC(C)(C)C)cc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
d6786c551347d89580cd19199d8055616f405cdef22ea256b5a523ba65083594
e024304228c7143d5ec452c855d5c53cce598d20ddcea996ef240d59c49deaa3
c1ccc(CSCCCC2CCNCC2)cc1
[C:1]-[C:2]-[CH;D2;+0:3]=[C;H0;D3;+0:4](-[C:5]-[C:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13].[SH;D1;+0:14]-[C:15]-[c:16]>>[C:1]-[C:2]-[CH;D3;+0:3](-[S;H0;D2;+0:14]-[C:15]-[c:16])-[CH;D3;+0:4](-[C:5]-[C:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13]
63
[{"value": 63.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CC(C(CC(C)C)SCC1=CC=C(C=C1)OC)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 63.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CC(C(CC(C)C)SCC1=CC=C(C=C1)OC)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 4-(2-tert-butoxycarbonyl-5-methyl-hex-2-enyl)-piperidine-1-carboxylic acid tert-butyl ester (2.0 g, 5.24 mmol) in DMF (5 mL) was added to a mixture of potassium carbonate (0.54 g, 3.93 mmol) and 4-methoxy-α-toluenethiol (1.17 g, 10.48 mmol) in DMF (50 mL) under nitrogen. The mixture was refluxed for 5 h a...
10.6084/m9.figshare.5104873.v1
null
Ester.Aliphatic thiol
Ester.Monosulfide
null
null
c1ccccc1.C1CC[NH]CC1
null
CN(C)C=O
null
null
CC(C)CC=C(CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OC(C)(C)C.COc1ccc(CS)cc1>CN(C)C=O>COc1ccc(CSC(CC(C)C)C(CC2CCN(C(=O)OC(C)(C)C)CC2)C(=O)OC(C)(C)C)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6952928057324816a1938954f85bcf59
CC(C)(C)OC(=O)C(=CCc1ccccc1)CC1CCN(C(=O)OC(C)(C)C)CC1.COc1ccc(CS)cc1>>COc1ccc(CSC(Cc2ccccc2)C(CC2CCN(C(=O)OC(C)(C)C)CC2)C(=O)OC(C)(C)C)cc1
O.C(C)(C)(C)OC(=O)N1CCC(CC1)CC(=CCC1=CC=CC=C1)C(=O)OC(C)(C)C.C([O-])([O-])=O.[K+].[K+].COC1=CC=C(C=C1)CS>>C(C)(C)(C)OC(=O)N1CCC(CC1)CC(C(CC1=CC=CC=C1)SCC1=CC=C(C=C1)OC)C(=O)OC(C)(C)C
[CH:9]([CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)=[C:17]([CH2:18][CH:19]1[CH2:20][CH2:21][N:22]([C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29])[CH2:30][CH2:31]1)[C:32](=[O:33])[O:34][C:35]([CH3:36])([CH3:37])[CH3:38].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][SH:8])[cH:39][cH:40]1>>[CH3:1][O:2][c:3]...
CC(C)(C)OC(=O)C(=CCc1ccccc1)CC1CCN(C(=O)OC(C)(C)C)CC1.COc1ccc(CS)cc1
COc1ccc(CSC(Cc2ccccc2)C(CC2CCN(C(=O)OC(C)(C)C)CC2)C(=O)OC(C)(C)C)cc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
d6786c551347d89580cd19199d8055616f405cdef22ea256b5a523ba65083594
e024304228c7143d5ec452c855d5c53cce598d20ddcea996ef240d59c49deaa3
c1ccc(CSC(CCC2CCNCC2)Cc2ccccc2)cc1
[C:1]-[C:2]-[C;H0;D3;+0:3](=[CH;D2;+0:4]-[C:5]-[c:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13].[SH;D1;+0:14]-[C:15]-[c:16]>>[C:1]-[C:2]-[CH;D3;+0:3](-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13])-[CH;D3;+0:4](-[C:5]-[c:6])-[S;H0;D2;+0:14]-[C:15]-[c:16]
50
[{"value": 50.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CC(C(CC1=CC=CC=C1)SCC1=CC=C(C=C1)OC)C(=O)OC(C)(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 50.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)CC(C(CC1=CC=CC=C1)SCC1=CC=C(C=C1)OC)C(=O)OC(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false...
75
CELSIUS
null
null
4-(2-tert-Butoxycarbonyl4-phenyl-but-2-enyl)-piperidine-1-carboxylic acid tert-butyl ester (0.8 g, 1.93 mmol) in DMF (10 mL) was added to a suspension of potassium carbonate (0.20 g, 1.44 mmol) ) and 4-methoxy-α-toluenethiol (0.54 mL, 3.85 mmol) in DMF (10 mL) under nitrogen. The mixture was heated to 75° C. for 24 h a...
10.6084/m9.figshare.5104873.v1
null
Ester.Aliphatic thiol
Ester.Monosulfide
null
null
c1ccccc1.c1ccccc1.C1CC[NH]CC1
null
CN(C)C=O
75
null
CC(C)(C)OC(=O)C(=CCc1ccccc1)CC1CCN(C(=O)OC(C)(C)C)CC1.COc1ccc(CS)cc1>CN(C)C=O>COc1ccc(CSC(Cc2ccccc2)C(CC2CCN(C(=O)OC(C)(C)C)CC2)C(=O)OC(C)(C)C)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4c91d3469d9e4eeeb3d52c80632ed8db
CCOCC.Cc1ccnc(N)c1>>CC(=O)Nc1cc(C)ccn1
NC1=NC=CC(=C1)C.C(C)OCC>>CC1=CC(=NC=C1)NC(C)=O
CC[O:3][CH2:2][CH3:1].[NH2:4][c:5]1[cH:6][c:7]([CH3:8])[cH:9][cH:10][n:11]1>>[CH3:1][C:2](=[O:3])[NH:4][c:5]1[cH:6][c:7]([CH3:8])[cH:9][cH:10][n:11]1
CCOCC.Cc1ccnc(N)c1
CC(=O)Nc1cc(C)ccn1
null
null
C(C)(=O)OC(C)=O
Acylation
OtherReaction
003d6e284475e7d4fe43f9e91e4ad7ca9bf4d7f2029a8fe4e8eed7dbde0fdef0
25423bd5162c5be916302ae1ac632b1f2d5d912d0ee7eadf1b5b1259507dc6c3
c1ccncc1
C-C-[O;H0;D2;+0:1]-[CH2;D2;+0:2]-[C;D1;H3:3].[NH2;D1;+0:4]-[c:5](:[c:6]):[#7;a:7]:[c:8]>>[C;D1;H3:3]-[C;H0;D3;+0:2](=[O;H0;D1;+0:1])-[NH;D2;+0:4]-[c:5](:[c:6]):[#7;a:7]:[c:8]
95
[{"value": 95.0, "product": "CC1=CC(=NC=C1)NC(C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Amino4-methylpyridine (99.0 g, 91.5 mmol) in acetic anhydride (250 mL) was warmed to 70° C. for two h. The mixture was cooled to room temperature and diethyl ether (100 mL) added. The product crystallized as white needle crystals. Filtering and drying in vacuo afforded N-(4-methyl-pyridin-2-yl)-acetamide (130 g, 95%)...
10.6084/m9.figshare.5104873.v1
null
Ether.Primary amine
Secondary amide
null
null
c1ccncc1
Other
C(C)(=O)OC(C)=O
null
null
CCOCC.Cc1ccnc(N)c1>C(C)(=O)OC(C)=O>CC(=O)Nc1cc(C)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cecb5bf832084ef5a6421240cee3dddf
CC(=O)Nc1cc(C(=O)O)ccn1.CCO>>CCOC(=O)c1ccnc(N)c1
C(C)(=O)NC=1C=C(C(=O)O)C=CN1.C(=O)(O)[O-].[Na+].C(C)O>>C(C)OC(C1=CC(=NC=C1)N)=O
CC(=O)[NH:11][c:10]1[n:9][cH:8][cH:7][c:6]([C:4](O)=[O:5])[cH:12]1.[CH3:1][CH2:2][OH:3]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][n:9][c:10]([NH2:11])[cH:12]1
CC(=O)Nc1cc(C(=O)O)ccn1.CCO
CCOC(=O)c1ccnc(N)c1
null
null
null
Acylation
OtherReaction
db4aad5bc6eb04613ddfb9a3aea41fadd2fa9a025207774fa644fb14d470fda3
1fa52715508855a72f553ab5455008c4c9437321a1b1d5fc5200958d9ee092d1
c1ccncc1
C-C(=O)-[NH;D2;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[c:5]:[c:6](-[C;H0;D3;+0:7](-O)=[O;D1;H0:8]):[c:9]:1.[C;D1;H3:10]-[C:11]-[OH;D1;+0:12]>>[C;D1;H3:10]-[C:11]-[O;H0;D2;+0:12]-[C;H0;D3;+0:7](=[O;D1;H0:8])-[c:6]1:[c:9]:[c:2](-[NH2;D1;+0:1]):[#7;a:3]:[c:4]:[c:5]:1
79
[{"value": 79.0, "product": "C(C)OC(C1=CC(=NC=C1)N)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylamino-isonicotinic acid (10.8 g, 60.0 mmol) was suspended in ethanol (150 mL) and BF3OEt2 (22 mL, 138 mmol) was added. The mixture was refluxed overnight, and after cooling to room temperature 10% NaHCO3 (250 mL) was added. The product was extracted with chloroform and the combined organic extracts were washed ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary amide.Primary alcohol
Ester.Primary amine
null
null
c1ccncc1
HO-
null
null
null
CC(=O)Nc1cc(C(=O)O)ccn1.CCO>>CCOC(=O)c1ccnc(N)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e22be225eb1c4553a6fd980d9b34a803
CCOC(=O)c1ccnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c1>>CC(C)(C)OC(=O)Nc1cc(CO)ccn1
C(C)OC(C1=CC(=NC=C1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>>C(C)(C)(C)OC(NC1=NC=CC(=C1)CO)=O
CCO[C:12]([c:11]1[cH:10][c:9]([N:8](C(=O)OC(C)(C)C)[C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[n:16][cH:15][cH:14]1)=[O:13]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][c:11]([CH2:12][OH:13])[cH:14][cH:15][n:16]1
CCOC(=O)c1ccnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c1
CC(C)(C)OC(=O)Nc1cc(CO)ccn1
null
null
C1CCOC1
Reduction
OtherReaction
20962d9bc1897de80b918f6efe4891a362b51f4c6f3af7bad47f6e2640fa482a
f7ff3a3ce995d934c8d2667c39df2283accf4ec6ad29f6be8bba5d4b604712d3
c1ccncc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3]1:[c:4]:[c:5](-[N;H0;D3;+0:6](-C(=O)-O-C(-C)(-C)-C)-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[C;D1;H3:13]):[#7;a:14]:[c:15]:[c:16]:1>>[C;D1;H3:11]-[C:10](-[C;D1;H3:12])(-[C;D1;H3:13])-[#8:9]-[C:7](=[O;D1;H0:8])-[NH;D2;+0:6]-[c:5]1:[#7;a:14]:[c:15]:[c:16]...
86.4
[{"value": 86.0, "product": "C(C)(C)(C)OC(NC1=NC=CC(=C1)CO)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.4, "product": "C(C)(C)(C)OC(NC1=NC=CC(=C1)CO)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of to 2-[N,N-bis(tert-Butoxycarbonyl)amino]-isonicotinic acid ethyl ester (35.0 g, 95.5 mmol) in THF (350 mL) was treated with LiAlH4 (7.25 g, 191 mmol) and refluxed for 1 h under nitrogen. The reaction mixture was poured carefully onto crushed ice and the product extracted several times with CHCl3 and CHCl3...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carbamic ester.Ester.Ether.Substituted dicarboximide.Boc
Carbamic ester.Primary alcohol
null
null
c1ccncc1
HO-
C1CCOC1
null
null
CCOC(=O)c1ccnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c1>C1CCOC1>CC(C)(C)OC(=O)Nc1cc(CO)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0d78069ce36d4a58bfce4e19432cccc4
BrC(Br)(Br)Br.CC(C)(C)OC(=O)Nc1cc(CO)ccn1>>CC(C)(C)OC(=O)Nc1cc(CBr)ccn1
C(C)(C)(C)OC(NC1=NC=CC(=C1)CO)=O.C1=CC=C(C=C1)P(C2=CC=CC=C2)C3=CC=CC=C3.C(Br)(Br)(Br)Br>>C(C)(C)(C)OC(NC1=NC=CC(=C1)CBr)=O
BrC(Br)(Br)[Br:13].O[CH2:12][c:11]1[cH:10][c:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[n:16][cH:15][cH:14]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][c:11]([CH2:12][Br:13])[cH:14][cH:15][n:16]1
BrC(Br)(Br)Br.CC(C)(C)OC(=O)Nc1cc(CO)ccn1
CC(C)(C)OC(=O)Nc1cc(CBr)ccn1
null
null
C(Cl)Cl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
c1ccncc1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[c:3]1:[c:4]:[c:5]:[#7;a:6]:[c:7]:[c:8]:1>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3]1:[c:4]:[c:5]:[#7;a:6]:[c:7]:[c:8]:1
82
[{"value": 82.0, "product": "C(C)(C)(C)OC(NC1=NC=CC(=C1)CBr)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.0, "product": "C(C)(C)(C)OC(NC1=NC=CC(=C1)CBr)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
(4-Hydroxymethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (8.00 g, 35.6 mmol) was dissolved in CH2Cl2 (150 mL) and treated with PPh3 (11.2 g, 42.8 mmol) under nitrogen. The reaction flask was cooled in an ice bath and CBr4 (14.2 g, 42.8 mmol) was added in small portions. The ice bath was removed after 30 min and th...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccncc1
HBr
C(Cl)Cl
null
8
BrC(Br)(Br)Br.CC(C)(C)OC(=O)Nc1cc(CO)ccn1>C(Cl)Cl>CC(C)(C)OC(=O)Nc1cc(CBr)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-805b1be0b06a48d0ae30146f8f6f791f
CC(C)(C)OC(=O)Nc1cc(CBr)ccn1.CCOC(=O)CC(=O)OCC>>CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
C(C)(C)(C)OC(NC1=NC=CC(=C1)CBr)=O.[H-].[Na+].C(CC(=O)OCC)(=O)OCC>>C(C)OC(C(C(=O)OCC)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O
Br[CH2:7][c:8]1[cH:9][cH:10][n:11][c:12]([NH:13][C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[cH:21]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:22](=[O:23])[O:24][CH2:25][CH3:26]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][cH:10][n:11][c:12]([NH:13][C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:1...
CC(C)(C)OC(=O)Nc1cc(CBr)ccn1.CCOC(=O)CC(=O)OCC
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
null
null
C1CCOC1
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
c1ccncc1
Br-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1.[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[CH2;D2;+0:12]-[C:13](=[O;D1;H0:14])-[#8:15]-[C:16]>>[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[CH;D3;+0:12](-[CH2;D2;+0:1]-[c:2]1:[c:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1)-[C:13](=[O;D1;H0:14])-[#8:15]-[C:16]
62.7
[{"value": 55.0, "product": "C(C)OC(C(C(=O)OCC)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.7, "product": "C(C)OC(C(C(=O)OCC)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a solution of NaH (80%, 0.17 g, 4.00 mmol) in THF (5 mL) at 0° C. under argon was added diethyl malonate (0.64 g, 4.00 mmol). After the mixture was stirred for 15 min the mixture was added to a refluxed mixture of (4-bromomethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.00 g, 3.48 mmol) in THF (10 mL), and the...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccncc1
HBr
C1CCOC1
null
0.25
CC(C)(C)OC(=O)Nc1cc(CBr)ccn1.CCOC(=O)CC(=O)OCC>C1CCOC1>CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d245cc3b73f8448fb111e6ba4a53d5dd
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC>>CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)O
[OH-].[K+].C(C)OC(C(C(=O)OCC)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O>>C(C)OC(C(C(=O)O)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O
CC[O:24][C:22]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][c:8]1[cH:9][cH:10][n:11][c:12]([NH:13][C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[cH:21]1)=[O:23]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][cH:10][n:11][c:12]([NH:13][C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[cH:...
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)O
null
null
C(Cl)Cl.C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
81.3
[{"value": 81.0, "product": "C(C)OC(C(C(=O)O)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 81.3, "product": "C(C)OC(C(C(=O)O)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of KOH (0.19 g, 3.43 mmol) in ethanol (5 mL) was added to a solution of 2-(2-tert-butoxycarbonylamino-pyridin4-ylmethyl)-malonic acid diethyl ester (1.20 g, 3.27 mmol) in ethanol (5 mL) and methylene chloride (5 mL) at 0° C. The mixture was stirred for 18 h at room temperature. The mixture was concentrated u...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1
Other
C(Cl)Cl.C(C)O
null
18
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC>C(Cl)Cl.C(C)O>CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d548d65a3035443ebaa3c97adc92d402
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)O>>C=C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
C(C)NCC.C(C)OC(C(C(=O)O)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O.C=O>>C(C)OC(C(=C)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O
O=[C:1](O)[CH:2]([CH2:3][c:4]1[cH:5][cH:6][n:7][c:8]([NH:9][C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[cH:17]1)[C:18](=[O:19])[O:20][CH2:21][CH3:22]>>[CH2:1]=[C:2]([CH2:3][c:4]1[cH:5][cH:6][n:7][c:8]([NH:9][C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[cH:17]1)[C:18](=[O:19])[O:20][CH2:21][CH3:22...
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)O
C=C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
485594ce7bba157615ffbb01ccede84a4e638576571b5d04649a06f3d4b7bce0
55e5b5078322f9f4fb0a7e9b5fc8a8cb9084e9135b447b8c441ad0800765792e
c1ccncc1
O-[C;H0;D3;+0:1](=O)-[CH;D3;+0:2](-[C:3]-[c:4])-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8]>>[C:8]-[#8:7]-[C:5](=[O;D1;H0:6])-[C;H0;D3;+0:2](=[CH2;D1;+0:1])-[C:3]-[c:4]
71.2
[{"value": 71.0, "product": "C(C)OC(C(=C)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 71.2, "product": "C(C)OC(C(=C)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
5
HOUR
A solution of diethylamine (0.26 g, 2.67 mmol) in methylene chloride (4 mL) was added to a mixture of 2-(2-tert-butoxycarbonylamino-pyridin4-ylmethyl)-malonic acid monoethyl ester (0.90 g, 2.66 mmol) and 37% aq. solution of formaldehyde (0.24 g, 3.00 mmol) at 0° C. The mixture was stirred for 5 h at room temperature an...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester.Vinyl
null
null
c1ccncc1
Other
C(Cl)Cl
null
5
CCOC(=O)C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)O>C(Cl)Cl>C=C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c5acf6150bfe4f35aa8cbad2307fd951
C=C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC.CC(O)=S>>CCOC(=O)C(CSC(C)=O)Cc1ccnc(NC(=O)OC(C)(C)C)c1
C(C)OC(C(=C)CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)=O.C(C)N(CC)CC.C(C)(=S)O>>C(C)OC(C(CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)CSC(C)=O)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[CH2:7])[CH2:12][c:13]1[cH:14][cH:15][n:16][c:17]([NH:18][C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[cH:26]1.[S:8]=[C:9]([CH3:10])[OH:11]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH2:12][c:13]1[cH:14][cH:15][n:16][c:17]([NH:18][C:19]...
C=C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC.CC(O)=S
CCOC(=O)C(CSC(C)=O)Cc1ccnc(NC(=O)OC(C)(C)C)c1
null
null
null
Protection
OtherReaction
56aa090d67fbecbea8a1963579cc34949775a09653b2b2f2795c609c60e70c77
5a9b0d631147b21b844b3c73866d1d81ab543538a176ebae28118ae7e39e572f
c1ccncc1
[C;D1;H3:1]-[C;H0;D3;+0:2](-[OH;D1;+0:3])=[S;H0;D1;+0:4].[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[C;H0;D3;+0:9](=[CH2;D1;+0:10])-[C:11]-[c:12]>>[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[CH;D3;+0:9](-[C:11]-[c:12])-[CH2;D2;+0:10]-[S;H0;D2;+0:4]-[C;H0;D3;+0:2](-[C;D1;H3:1])=[O;H0;D1;+0:3]
100
[{"value": 100.0, "product": "C(C)OC(C(CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A solution of 2-(2-tert-butoxycarbonylamino-pyridin-4-ylmethyl)-acrylic acid ethyl ester (0.48 g, 1.57 mmol) and triethylamine (0.17 g, 1.64 mmol) was added to thioacetic acid (3 mL) at 0° C. under nitrogen. The mixture was stirred at room temperature for 4 h. The mixture was poured onto ice-water and extracted with CH...
10.6084/m9.figshare.5104873.v1
null
Ester.Thiocarbonyl.Vinyl
Ester.Carbo-thioester
null
null
c1ccncc1
null
null
null
4
C=C(Cc1ccnc(NC(=O)OC(C)(C)C)c1)C(=O)OCC.CC(O)=S>>CCOC(=O)C(CSC(C)=O)Cc1ccnc(NC(=O)OC(C)(C)C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6e298fbb1394474fb21851f588a962f4
CCOC(=O)C(CSC(C)=O)Cc1ccnc(NC(=O)OC(C)(C)C)c1>>CCOC(=O)C(CSC(C)=O)Cc1ccnc(N)c1
C(=O)(C(F)(F)F)O.C(C)OC(C(CC1=CC(=NC=C1)NC(=O)OC(C)(C)C)CSC(C)=O)=O>>C(C)OC(C(CC1=CC(=NC=C1)N)CSC(C)=O)=O
CC(C)(C)OC(=O)[NH:18][c:17]1[n:16][cH:15][cH:14][c:13]([CH2:12][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][S:8][C:9]([CH3:10])=[O:11])[cH:19]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH2:12][c:13]1[cH:14][cH:15][n:16][c:17]([NH2:18])[cH:19]1
CCOC(=O)C(CSC(C)=O)Cc1ccnc(NC(=O)OC(C)(C)C)c1
CCOC(=O)C(CSC(C)=O)Cc1ccnc(N)c1
null
null
C(Cl)Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]
141.7
[{"value": 100.0, "product": "C(C)OC(C(CC1=CC(=NC=C1)N)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 141.7, "product": "C(C)OC(C(CC1=CC(=NC=C1)N)CSC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
60
MINUTE
TFA (0.5 mL) was added to a solution of 2-acetylsulfanylmethyl-3-(2-tert-butoxycarbonylamino-pyridin4-yl)-propionic acid ethyl ester (50 mg, 0.13 mmol) in methylene chloride under argon. The solution was stirred for 60 min and concentrated under reduced pressure to give crude 2-acetylsulfanylmethyl-3-(2-amino-pyridin-4...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccncc1
HO-
C(Cl)Cl
null
1
CCOC(=O)C(CSC(C)=O)Cc1ccnc(NC(=O)OC(C)(C)C)c1>C(Cl)Cl>CCOC(=O)C(CSC(C)=O)Cc1ccnc(N)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4bf3e9ebafb04352b1ad44652b3c3909
CCOC(=O)C(CSC(C)=O)Cc1ccnc(N)c1>>Nc1cc(CC(CS)C(=O)O)ccn1
C(C)OC(C(CC1=CC(=NC=C1)N)CSC(C)=O)=O>>NC1=NC=CC(=C1)CC(C(=O)O)CS
CC[O:11][C:9]([CH:6]([CH2:5][c:4]1[cH:3][c:2]([NH2:1])[n:14][cH:13][cH:12]1)[CH2:7][S:8]C(C)=O)=[O:10]>>[NH2:1][c:2]1[cH:3][c:4]([CH2:5][CH:6]([CH2:7][SH:8])[C:9](=[O:10])[OH:11])[cH:12][cH:13][n:14]1
CCOC(=O)C(CSC(C)=O)Cc1ccnc(N)c1
Nc1cc(CC(CS)C(=O)O)ccn1
null
null
Cl
Reduction
OtherReaction
1bcd8cbb2f136b4bcba1690e9ba45c4e43c89ba76f0e22de82a7d3fe318c82a9
5654c46fe4cb226f88ec3c899c7f9be1825c357673ea686958f9ef4883ee1db3
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[S;H0;D2;+0:6]-C(-C)=O>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[C:4]-[C:5]-[SH;D1;+0:6]
100
[{"value": 100.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylsulfanylmethyl-3-(2-amino-pyridin4-yl)-propionic acid ethyl ester (52 mg, 0.13 mmol) was dissolved in conc. HCl (2 mL) under argon. The solution was heated to reflux for 1 h. Concentration under reduced pressure gave the title compound as the hydrochloride salt (32 mg, 100%). Conditions: See reaction.notes.proc...
10.6084/m9.figshare.5104873.v1
null
Ester.Carbo-thioester
Carboxylic acid.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
null
CCOC(=O)C(CSC(C)=O)Cc1ccnc(N)c1>Cl>Nc1cc(CC(CS)C(=O)O)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a2acfb645bed42be8eb04a3e474dcc98
CCOCC.Nc1ccc(C(=O)O)cn1>>CCOC(=O)c1ccc(N)nc1
NC1=NC=C(C=C1)C(=O)O.[OH-].[Na+].C(C)OCC.O=S(Cl)Cl.O=S(Cl)Cl.O=S(Cl)Cl>>C(C)OC(C1=CN=C(C=C1)N)=O
CCO[CH2:2][CH3:1].[OH:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH2:10])[n:11][cH:12]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][cH:8][c:9]([NH2:10])[n:11][cH:12]1
CCOCC.Nc1ccc(C(=O)O)cn1
CCOC(=O)c1ccc(N)nc1
null
null
C1CCOC1.CO.C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
51b8a6656c0a2b883c9ef3d6e10f16e7a23403a54025d10a356d536fd60cd751
c9da2d501363e26e3362b4d92445c316ae4db0a7128a4caa823650c7a4fa5893
c1ccncc1
C-C-O-[CH2;D2;+0:1]-[C;D1;H3:2].[#7;a:3]:[c:4]:[c:5]-[C:6](=[O;D1;H0:7])-[OH;D1;+0:8]>>[#7;a:3]:[c:4]:[c:5]-[C:6](=[O;D1;H0:7])-[O;H0;D2;+0:8]-[CH2;D2;+0:1]-[C;D1;H3:2]
97
[{"value": 97.0, "product": "C(C)OC(C1=CN=C(C=C1)N)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
2-Amino-5-pyridinecarboxylic acid (25.0 g, 181 mmol) was suspended in ethanol (190 mL) and SOCl2 (15 mL, 206 mmol) was added. The mixture was refluxed for 10 hs and more SOCl2 (16 mL) was added. After 3 days with reflux (and more SOCl2 (10 mL) added each day), the reaction mixture was cooled to room temperature and die...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether
Ester
null
null
c1ccncc1
HO-
C1CCOC1.CO.C(C)O
null
1
CCOCC.Nc1ccc(C(=O)O)cn1>C1CCOC1.CO.C(C)O>CCOC(=O)c1ccc(N)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-974d6f3d98044b19b9a4be784b331090
CCOC(=O)c1ccc(NC(=O)OC(C)(C)C)nc1>>CC(C)(C)OC(=O)Nc1ccc(CO)cn1
C(C)OC(C1=CN=C(C=C1)NC(=O)OC(C)(C)C)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3].[NH4+].[Cl-]>>C(C)(C)(C)OC(NC1=NC=C(C=C1)CO)=O
CCO[C:13]([c:12]1[cH:11][cH:10][c:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[n:16][cH:15]1)=[O:14]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][cH:11][c:12]([CH2:13][OH:14])[cH:15][n:16]1
CCOC(=O)c1ccc(NC(=O)OC(C)(C)C)nc1
CC(C)(C)OC(=O)Nc1ccc(CO)cn1
null
null
C1CCOC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccncc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
68.1
[{"value": 68.0, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)CO)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 68.1, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)CO)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
6
HOUR
To a stirred solution of 6-tert-butoxycarbonylamino-nicotinic acid ethyl ester (3.50 g, 13.1 mmol) in THF (20 mL) under nitrogen was added LiAlH4 (0.91 g, 24.0 mmol) in THF (20 mL) over a period of 2 h. The reaction mixture was stirred for 6 h, then NH4Cl (sat.) was added (carefully) until neutral solution. The mixture...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccncc1
HO-
C1CCOC1
null
6
CCOC(=O)c1ccc(NC(=O)OC(C)(C)C)nc1>C1CCOC1>CC(C)(C)OC(=O)Nc1ccc(CO)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-40c9ef8798c5405c862f433fe954dac4
BrC(Br)(Br)Br.CC(C)(C)OC(=O)Nc1ccc(CO)cn1>>CC(C)(C)OC(=O)Nc1ccc(CBr)cn1
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(Br)(Br)(Br)Br.C(C)(C)(C)OC(NC1=NC=C(C=C1)CO)=O>>C(C)(C)(C)OC(NC1=NC=C(C=C1)CBr)=O
BrC(Br)(Br)[Br:14].O[CH2:13][c:12]1[cH:11][cH:10][c:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[n:16][cH:15]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][cH:11][c:12]([CH2:13][Br:14])[cH:15][n:16]1
BrC(Br)(Br)Br.CC(C)(C)OC(=O)Nc1ccc(CO)cn1
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1
null
null
C(Cl)Cl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
c1ccncc1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
67
[{"value": 67.0, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)CBr)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 66.5, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)CBr)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-20
CELSIUS
5
HOUR
Triphenylphosphine (8.70 g, 33.1 mmol) and carbontetrabromide (17.0 g, 51.2 mmol) were added to a suspension of (5-hydroxymethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (7.00 g 31.2 mmol) in CH2Cl2 (200 mL) at room temperature. Stirring was continued for 5 h followed by evaporation of the solvent. Acetonitrile (20...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccncc1
HBr
C(Cl)Cl
-20
5
BrC(Br)(Br)Br.CC(C)(C)OC(=O)Nc1ccc(CO)cn1>C(Cl)Cl>CC(C)(C)OC(=O)Nc1ccc(CBr)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fdd178d6b86e4eb282f637ab9c2a16a5
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCOC(=O)CC(=O)OCC>>CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
C(C)(C)(C)OC(NC1=NC=C(C=C1)CBr)=O.[H-].[Na+].C(CC(=O)OCC)(=O)OCC>>C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
Br[CH2:7][c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:21]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:22](=[O:23])[O:24][CH2:25][CH3:26]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH...
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCOC(=O)CC(=O)OCC
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
null
null
C1CCOC1
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
c1ccncc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
44
[{"value": 44.0, "product": "C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 43.7, "product": "C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a suspension of NaH (0.49 g, 16.3 mmol, 80%) in THF (15 mL) at 0° C. was added diethyl malonate (2.61 g, 16.3 mmol). The mixture was stirred for 15 min and was then added dropwise to a refluxed mixture of (5-bromomethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (3.90 g, 13.6 mmol) in THF (25 mL), and the resultin...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccncc1
HBr
C1CCOC1
null
0.25
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCOC(=O)CC(=O)OCC>C1CCOC1>CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-dcc7ced14d924601a79f1709878a8ac1
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC>>CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O
[OH-].[K+].C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O>>C(C)OC(C(C(=O)O)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
CC[O:24][C:22]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:21]1)=[O:23]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:...
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O
null
null
C(Cl)Cl.C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
50
[{"value": 50.0, "product": "C(C)OC(C(C(=O)O)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 49.7, "product": "C(C)OC(C(C(=O)O)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of KOH (0.37 g, 6.54 mmol) in ethanol (5 mL) was added to a solution of 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-malonic acid diethyl ester (2.18 g, 5.95 mmol) in ethanol (25 mL) and methylene chloride (10 mL) at 0° C. The mixture was stirred for 18 h at room temperature. The mixture was concentrate...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1
Other
C(Cl)Cl.C(C)O
null
18
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC>C(Cl)Cl.C(C)O>CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2f8a6931a93f483288158d8ee6690ca6
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O>>C=C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
C(C)NCC.O.C(C)OC(C(C(=O)O)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.C=O>>C(C)OC(C(=C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
O=[C:1](O)[CH:2]([CH2:3][c:4]1[cH:5][cH:6][c:7]([NH:8][C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[n:16][cH:17]1)[C:18](=[O:19])[O:20][CH2:21][CH3:22]>>[CH2:1]=[C:2]([CH2:3][c:4]1[cH:5][cH:6][c:7]([NH:8][C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[n:16][cH:17]1)[C:18](=[O:19])[O:20][CH2:21][CH3:22...
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O
C=C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
485594ce7bba157615ffbb01ccede84a4e638576571b5d04649a06f3d4b7bce0
55e5b5078322f9f4fb0a7e9b5fc8a8cb9084e9135b447b8c441ad0800765792e
c1ccncc1
O-[C;H0;D3;+0:1](=O)-[CH;D3;+0:2](-[C:3]-[c:4]:[c:5]:[#7;a:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]>>[#7;a:6]:[c:5]:[c:4]-[C:3]-[C;H0;D3;+0:2](=[CH2;D1;+0:1])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]
83
[{"value": 83.0, "product": "C(C)OC(C(=C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.7, "product": "C(C)OC(C(=C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Diethylamine (0.29 g, 3.00 mmol), water (2 mL) and methylene chloride (2 mL) was added to a mixture of 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-malonic acid monoethyl ester (1.00 g, 2.96 mmol) and 37% aq. solution of formaldehyde (0.25 g, 3.05 mmol) at 0° C. The mixture was stirred for 16 h at room temperature...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester.Vinyl
null
null
c1ccncc1
Other
C(Cl)Cl
null
16
CCOC(=O)C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O>C(Cl)Cl>C=C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-96d8d198c68c43a1930af17b5b4a14c6
C=C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC.CC(O)=S>>CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
C(C)OC(C(=C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.C(C)N(CC)CC.C(C)(=S)O>>C(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[CH2:7])[CH2:12][c:13]1[cH:14][cH:15][c:16]([NH:17][C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[n:25][cH:26]1.[S:8]=[C:9]([CH3:10])[OH:11]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH2:12][c:13]1[cH:14][cH:15][c:16]([NH:17][C:18](=[O:1...
C=C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC.CC(O)=S
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
null
null
null
Protection
OtherReaction
56aa090d67fbecbea8a1963579cc34949775a09653b2b2f2795c609c60e70c77
5a9b0d631147b21b844b3c73866d1d81ab543538a176ebae28118ae7e39e572f
c1ccncc1
[#7;a:1]:[c:2]:[c:3]-[C:4]-[C;H0;D3;+0:5](=[CH2;D1;+0:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10].[C;D1;H3:11]-[C;H0;D3;+0:12](-[OH;D1;+0:13])=[S;H0;D1;+0:14]>>[#7;a:1]:[c:2]:[c:3]-[C:4]-[CH;D3;+0:5](-[CH2;D2;+0:6]-[S;H0;D2;+0:14]-[C;H0;D3;+0:12](-[C;D1;H3:11])=[O;H0;D1;+0:13])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]
61
[{"value": 61.0, "product": "C(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
6
HOUR
2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-acrylic acid ethyl ester (0.49 g, 1.60 mmol) and triethylamine (0.17 g, 1.64 mmol) were added to thioacetic acid (3 mL) at 0° C. The mixture was stirred at room temperature for 6 h. The mixture was poured onto ice-water and extracted with CH2Cl2. The organic phase was w...
10.6084/m9.figshare.5104873.v1
null
Ester.Thiocarbonyl.Vinyl
Ester.Carbo-thioester
null
null
c1ccncc1
null
null
null
6
C=C(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC.CC(O)=S>>CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0f68fb696f96473182b690e0a2a91214
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1>>CCOC(=O)C(CSC(C)=O)Cc1ccc(N)nc1
C(=O)(C(F)(F)F)O.C(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O>>C(C)OC(C(CC=1C=NC(=CC1)N)CSC(C)=O)=O
CC(C)(C)OC(=O)[NH:17][c:16]1[cH:15][cH:14][c:13]([CH2:12][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][S:8][C:9]([CH3:10])=[O:11])[cH:19][n:18]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH2:12][c:13]1[cH:14][cH:15][c:16]([NH2:17])[n:18][cH:19]1
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
CCOC(=O)C(CSC(C)=O)Cc1ccc(N)nc1
null
null
C(Cl)Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]
141.7
[{"value": 100.0, "product": "C(C)OC(C(CC=1C=NC(=CC1)N)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 141.7, "product": "C(C)OC(C(CC=1C=NC(=CC1)N)CSC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
60
MINUTE
TFA (0.5 mL) was added to a solution of 2-acetylsulfanylmethyl-3-(6-tert-butoxycarbonylaminopyridin-3-yl)-propionic acid ethyl ester (100 mg, 0.26 mmol) in methylene chloride (2 mL) under argon. The solution was stirred for 60 min and concentrated under reduced pressure to give crude 2-acetylsulfanylmethyl-3-(6-amino-p...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccncc1
HO-
C(Cl)Cl
null
1
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1>C(Cl)Cl>CCOC(=O)C(CSC(C)=O)Cc1ccc(N)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c422c5c80ac74dc8a85345718451f205
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1>>Nc1ccc(CC(CS)C(=O)O)cn1
C(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O>>NC1=CC=C(C=N1)CC(C(=O)O)CS
CC[O:12][C:10]([CH:7]([CH2:6][c:5]1[cH:4][cH:3][c:2]([NH:1]C(=O)OC(C)(C)C)[n:14][cH:13]1)[CH2:8][S:9]C(C)=O)=[O:11]>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([CH2:6][CH:7]([CH2:8][SH:9])[C:10](=[O:11])[OH:12])[cH:13][n:14]1
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
Nc1ccc(CC(CS)C(=O)O)cn1
null
null
Cl
Reduction
OtherReaction
df63f36502c6e187beb1211487c3f0937031934a12a3c506c12c51a17b700a31
9a7c4efef36aa8beb2b85c58cd3924b350f3ef529d4eb0778d927167159d9d8b
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].C-C-[O;H0;D2;+0:6]-[C:7](=[O;D1;H0:8])-[C:9]-[C:10]-[S;H0;D2;+0:11]-C(-C)=O>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[O;D1;H0:8]=[C:7](-[OH;D1;+0:6])-[C:9]-[C:10]-[SH;D1;+0:11]
126.1
[{"value": 100.0, "product": "NC1=CC=C(C=N1)CC(C(=O)O)CS", "details": "PERCENTYIELD", "is_desired": false}, {"value": 126.1, "product": "NC1=CC=C(C=N1)CC(C(=O)O)CS", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
2-Acetylsulfanylmethyl-3-(6-tert-butoxycarbonylamino-pyridin-3-yl)-propionic acid ethyl ester (38 mg, 0.096 mmol) was dissolved in conc. HCl (2.0 mL) under argon. The solution was stirred at room temperature for 1 h and then heated to reflux for 1 h. Concentration under reduced pressure gave the title compound (25.7 mg...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Ether.Carbo-thioester.Boc
Carboxylic acid.Primary amine.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
1
CCOC(=O)C(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1>Cl>Nc1ccc(CC(CS)C(=O)O)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f8a92e98d3404dbf8bf128e5eee8b1de
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCOC(=O)C(C)C(=O)OC(C)(C)C>>CCOC(=O)C(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C
CCOC(=O)C.CC(C(=O)OC(C)(C)C)C(=O)OCC.[H-].[Na+].C(C)(C)(C)OC(NC1=NC=C(C=C1)CBr)=O>>C(C)OC(C(C(=O)OC(C)(C)C)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
Br[CH2:8][c:9]1[cH:10][cH:11][c:12]([NH:13][C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[n:21][cH:22]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH3:7])[C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH2:8][c:9]1[cH:10][cH:11][c:12]([NH:13][C:14](=[O:15]...
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCOC(=O)C(C)C(=O)OC(C)(C)C
CCOC(=O)C(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C
null
null
CCCCCCC.CCOC(=O)C.CN(C)C=O
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
c1ccncc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[C;D1;H3:12])-[C:13](=[O;D1;H0:14])-[#8:15]-[C:16](-[C;D1;H3:17])(-[C;D1;H3:18])-[C;D1;H3:19]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[C;H0;D4;+0:11](-[C;D1;H3:12])(-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:13](=...
61.5
[{"value": 61.0, "product": "C(C)OC(C(C(=O)OC(C)(C)C)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.5, "product": "C(C)OC(C(C(=O)OC(C)(C)C)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
A solution of tert-butyl ethyl methylmalonate (457 mg, 2.26 mmol) in DMF (4 mL) was added dropwise to a suspension of NaH (90 mg, 2.26 mmol, 60% in oil) in DMF (4 mL). The reaction mixture was stirred for 20 min. A solution of (5-bromomethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (500 mg, 1.74 mmol) in DMF (2.5 m...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccncc1
HBr
CCCCCCC.CCOC(=O)C.CN(C)C=O
null
0.333333
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCOC(=O)C(C)C(=O)OC(C)(C)C>CCCCCCC.CCOC(=O)C.CN(C)C=O>CCOC(=O)C(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b21262ed18ac45b1b012ac9c43caf368
CCOC(=O)C(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C>>CC(C)(C)OC(=O)Nc1ccc(CC(C)(C(=O)O)C(=O)OC(C)(C)C)cn1
[OH-].[Na+].C(C)OC(C(C(=O)OC(C)(C)C)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.C(Cl)Cl>>C(C)(C)(C)OC(C(C(=O)O)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
CC[O:18][C:16]([C:14]([CH2:13][c:12]1[cH:11][cH:10][c:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[n:27][cH:26]1)([CH3:15])[C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])=[O:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][cH:11][c:12]([CH2:13][C:14]([CH3:15])([C:16](=[O:1...
CCOC(=O)C(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C
CC(C)(C)OC(=O)Nc1ccc(CC(C)(C(=O)O)C(=O)OC(C)(C)C)cn1
null
null
C1CCOC1.CCO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
89
[{"value": 89.0, "product": "C(C)(C)(C)OC(C(C(=O)O)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.8, "product": "C(C)(C)(C)OC(C(C(=O)O)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
16
HOUR
1M NaOH (2 mL) was added to a solution of 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-2-methyl-malonic acid tert-butyl ester ethyl ester (0.42g, 1.03 mmol) in THF/EtOH (4 mL, 1:1) . The reaction mixture was stirred at 50° C. for 16 h. CH2Cl2 was added and the mixture was washed with 0.5 M HCl and brine and dried....
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1
Other
C1CCOC1.CCO
50
16
CCOC(=O)C(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C>C1CCOC1.CCO>CC(C)(C)OC(=O)Nc1ccc(CC(C)(C(=O)O)C(=O)OC(C)(C)C)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-33705ed7c39b4002b3186b0f5b799ade
CC(C)(C)OC(=O)Nc1ccc(CC(C)(C(=O)O)C(=O)OC(C)(C)C)cn1>>CC(C)(C)OC(=O)Nc1ccc(CC(C)(CO)C(=O)OC(C)(C)C)cn1
[BH4-].[Na+].ClC(=O)OC.C(C)(C)(C)OC(C(C(=O)O)(C)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.CCN(CC)CC.Cl>>C(C)(C)(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)(C)CO)=O
O=[C:16]([C:14]([CH2:13][c:12]1[cH:11][cH:10][c:9]([NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[n:26][cH:25]1)([CH3:15])[C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[OH:17]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][cH:11][c:12]([CH2:13][C:14]([CH3:15])([CH2:16][OH:17])[C...
CC(C)(C)OC(=O)Nc1ccc(CC(C)(C(=O)O)C(=O)OC(C)(C)C)cn1
CC(C)(C)OC(=O)Nc1ccc(CC(C)(CO)C(=O)OC(C)(C)C)cn1
null
null
CCOC(=O)C.C1CCOC1
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
c1ccncc1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[C:3](-[C:4])(-[C;D1;H3:5])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12]>>[C:4]-[C:3](-[C;D1;H3:5])(-[CH2;D2;+0:1]-[O;D1;H1:2])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[C;D1;H3:12]
57
[{"value": 57.0, "product": "C(C)(C)(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)(C)CO)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 56.7, "product": "C(C)(C)(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)(C)CO)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
Methyl chloroformate (75 μL, 0.92 mmol) was added dropwise to a solution of 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-2-methyl-malonic acid mono-tert-butyl ester (348 mg, 0.915 mmol) and Et3N (123 μL, 0.92 mmol) in THF (6 mL). The reaction mixture was stirred for 20 min., filtered and added dropwise to a suspen...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
c1ccncc1
Other
CCOC(=O)C.C1CCOC1
null
0.333333
CC(C)(C)OC(=O)Nc1ccc(CC(C)(C(=O)O)C(=O)OC(C)(C)C)cn1>CCOC(=O)C.C1CCOC1>CC(C)(C)OC(=O)Nc1ccc(CC(C)(CO)C(=O)OC(C)(C)C)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e888b47742fc4305b15e5deb0b2c9806
CC(=O)SCC(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C>>CC(CS)(Cc1ccc(N)nc1)C(=O)O
C(C)(C)(C)OC(C(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)(C)CSC(C)=O)=O>>NC1=CC=C(C=N1)CC(C(=O)O)(C)CS
CC(=O)[S:4][CH2:3][C:2]([CH3:1])([CH2:5][c:6]1[cH:7][cH:8][c:9]([NH:10]C(=O)OC(C)(C)C)[n:11][cH:12]1)[C:13](=[O:14])[O:15]C(C)(C)C>>[CH3:1][C:2]([CH2:3][SH:4])([CH2:5][c:6]1[cH:7][cH:8][c:9]([NH2:10])[n:11][cH:12]1)[C:13](=[O:14])[OH:15]
CC(=O)SCC(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C
CC(CS)(Cc1ccc(N)nc1)C(=O)O
null
null
Cl
Reduction
OtherReaction
a39c0c4dba61501662345cdda2d7f368bc5e8fadffcb633e88bc3f6ed0e54457
27913482120c0868f0c9d959294323fb2e143509e943c964b43b532c74e3e01c
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].C-C(=O)-[S;H0;D2;+0:6]-[C:7]-[C:8]-[C:9](=[O;D1;H0:10])-[O;H0;D2;+0:11]-C(-C)(-C)-C>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[O;D1;H0:10]=[C:9](-[OH;D1;+0:11])-[C:8]-[C:7]-[SH;D1;+0:6]
100
[{"value": 100.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylsulfanylmethyl-3-(6-tert-butoxycarbonylamino-pyridin-3-yl)-2-methyl-propionic acid tert-butyl ester (4 mg, 9.4 μmol) was dissolved in conc. HCl under argon. The solution was heated to reflux for 1 h. Concentration under reduced pressure yielded the title compound as the hydrochloride salt (2.5 mg, 100%). Condit...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Ether.Carbo-thioester.Boc.Boc
Carboxylic acid.Primary amine.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
null
CC(=O)SCC(C)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OC(C)(C)C>Cl>CC(CS)(Cc1ccc(N)nc1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-436afded2b2d4ff79d62622977886f08
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCC1C(=O)OC(C)(C)OC1=O>>CCC1(Cc2ccc(NC(=O)OC(C)(C)C)nc2)C(=O)OC(C)(C)OC1=O
O.C(C)(C)(C)OC(NC1=NC=C(C=C1)CBr)=O.CC1(OC(C(C(O1)=O)CC)=O)C.C(C)N(CC)CC>>C(C)(C)(C)OC(NC1=NC=C(C=C1)CC1(C(OC(OC1=O)(C)C)=O)CC)=O
Br[CH2:4][c:5]1[cH:6][cH:7][c:8]([NH:9][C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[n:17][cH:18]1.[CH3:1][CH2:2][CH:3]1[C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[O:25][C:26]1=[O:27]>>[CH3:1][CH2:2][C:3]1([CH2:4][c:5]2[cH:6][cH:7][c:8]([NH:9][C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[n:17]...
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCC1C(=O)OC(C)(C)OC1=O
CCC1(Cc2ccc(NC(=O)OC(C)(C)C)nc2)C(=O)OC(C)(C)OC1=O
null
null
CS(=O)C
C-C Coupling
OtherReaction
58c01b66b8fc3a6ba5c7ea5eb9ff9622f5543ddf5dc16015d0c2c6736b592a81
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
O=C1OCOC(=O)C1Cc1cccnc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C;D1;H3:7]-[C:8]-[CH;D3;+0:9]1-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]-[#8:14]-[C:15]-1=[O;D1;H0:16]>>[C;D1;H3:7]-[C:8]-[C;H0;D4;+0:9]1(-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]-[#8:14]-[C:15]-1=[O;D1;H0:16]
87.3
[{"value": 87.0, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)CC1(C(OC(OC1=O)(C)C)=O)CC)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.3, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)CC1(C(OC(OC1=O)(C)C)=O)CC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
(5-Bromomethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.0 g, 3.48 mmol) was added to a solution of 2,2-dimethyl-5-ethyl-1,3-dioxane4,6-dione (600 mg, 3.48 mmol) and triethylamine (0.51 mL, 3.66 mmol) in dimethyl sulfoxide (40 mL) under nitrogen. The reaction mixture was stirred over night and water (100 mL) was ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
C1COCOC1
C1COCOC1
c1ccncc1.C1COCOC1
HBr
CS(=O)C
null
null
CC(C)(C)OC(=O)Nc1ccc(CBr)cn1.CCC1C(=O)OC(C)(C)OC1=O>CS(=O)C>CCC1(Cc2ccc(NC(=O)OC(C)(C)C)nc2)C(=O)OC(C)(C)OC1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eecf4b8b12244c0d82a0c50d09c6c711
CCOC(=O)C(CC)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O>>CCOC(=O)C(CC)(CO)Cc1ccc(NC(=O)OC(C)(C)C)nc1
[BH4-].[Na+].ClC(=O)OC.C(C)OC(C(C(=O)O)(CC)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.CCN(CC)CC.Cl>>C(C)OC(C(CC)(CO)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
O=[C:9]([C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH2:7][CH3:8])[CH2:11][c:12]1[cH:13][cH:14][c:15]([NH:16][C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[n:24][cH:25]1)[OH:10]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH2:7][CH3:8])([CH2:9][OH:10])[CH2:11][c:12]1[cH:13][cH:14][c:15]([NH:16][C:17](=[O:18])[O:19][...
CCOC(=O)C(CC)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O
CCOC(=O)C(CC)(CO)Cc1ccc(NC(=O)OC(C)(C)C)nc1
null
null
C(Cl)Cl.C1CCOC1
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
c1ccncc1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[C:3](-[C:4])(-[C:5])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9]>>[C:4]-[C:3](-[C:5])(-[CH2;D2;+0:1]-[O;D1;H1:2])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9]
45
[{"value": 45.0, "product": "C(C)OC(C(CC)(CO)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 44.6, "product": "C(C)OC(C(CC)(CO)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
50
MINUTE
Methyl chloroformate (150 pL, 1.95 mmol) was added dropwise to a solution of 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-2-ethyl-malonic acid monoethyl ester (700 mg, 1.91 mmol) and Et3N (275 μL, 1.97 mmol) in THF (15 mL) at −20° C. under nitrogen. The reaction mixture was stirred for 50 min., filtered and added ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
c1ccncc1
Other
C(Cl)Cl.C1CCOC1
null
0.833333
CCOC(=O)C(CC)(Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)O>C(Cl)Cl.C1CCOC1>CCOC(=O)C(CC)(CO)Cc1ccc(NC(=O)OC(C)(C)C)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c7bfad46cf2d45ad9426ac70adf14b9c
CCOC(=O)C(CC)(CO)Cc1ccc(NC(=O)OC(C)(C)C)nc1.O=C(O)Cc1cccs1>>CCOC(=O)C(CC)(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
N(=NC(=O)OC(C)C)C(=O)OC(C)C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.S1C(=CC=C1)CC(=O)O.C(C)OC(C(CC)(CO)CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O>>C(C)OC(C(CC)(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O
O[CH2:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH2:7][CH3:8])[CH2:14][c:15]1[cH:16][cH:17][c:18]([NH:19][C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[n:27][cH:28]1.OC([CH2:12][c:11]1ccc[s:10]1)=[O:13]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH2:7][CH3:8])([CH2:9][S:10][C:11]([CH3:12])=[O:13])[CH2:14][c:15]...
CCOC(=O)C(CC)(CO)Cc1ccc(NC(=O)OC(C)(C)C)nc1.O=C(O)Cc1cccs1
CCOC(=O)C(CC)(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
null
null
C1CCOC1
Protection
OtherReaction
189263d4d19565b9c5c001a81e8abf2a60b1807919ec489920cd4293a1993653
7a83c40990eef465e85ff66652874583517e7c7b69d7750d5f2438fef535f94e
c1ccncc1
O-C(=[O;H0;D1;+0:1])-[CH2;D2;+0:2]-[c;H0;D3;+0:3]1:[s;H0;D2;+0:4]:c:c:c:1.O-[CH2;D2;+0:5]-[C:6](-[C:7])(-[C:8])-[C:9](=[O;D1;H0:10])-[#8:11]-[C:12]>>[C:7]-[C:6](-[C:8])(-[CH2;D2;+0:5]-[S;H0;D2;+0:4]-[C;H0;D3;+0:3](-[CH3;D1;+0:2])=[O;H0;D1;+0:1])-[C:9](=[O;D1;H0:10])-[#8:11]-[C:12]
61.1
[{"value": 61.0, "product": "C(C)OC(C(CC)(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 61.1, "product": "C(C)OC(C(CC)(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Diisopropyl azodicarboxylate (296 μL, 1.53 mmol) was added dropwise to a solution of triphenylphosphine (402 mg, 1.53 mmol) in THF (4 mL) at 0° C. under argon and the reaction was stirred for 30 min. A solution of thiolacetic acid (109 μL, 1.53 mmol) and 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-2-hydroxymethyl...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary alcohol
Carbo-thioester
c1ccsc1
null
c1ccncc1
HO-
C1CCOC1
null
0.5
CCOC(=O)C(CC)(CO)Cc1ccc(NC(=O)OC(C)(C)C)nc1.O=C(O)Cc1cccs1>C1CCOC1>CCOC(=O)C(CC)(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cfa2598c674d45cd8384f953ab1e1107
CCOC(=O)C(CC)(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1>>CCC(CS)(Cc1ccc(N)nc1)C(=O)O
C(C)OC(C(CC)(CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)CSC(C)=O)=O>>NC1=CC=C(C=N1)CC(C(=O)O)(CC)CS
CC[O:16][C:14]([C:3]([CH2:2][CH3:1])([CH2:4][S:5]C(C)=O)[CH2:6][c:7]1[cH:8][cH:9][c:10]([NH:11]C(=O)OC(C)(C)C)[n:12][cH:13]1)=[O:15]>>[CH3:1][CH2:2][C:3]([CH2:4][SH:5])([CH2:6][c:7]1[cH:8][cH:9][c:10]([NH2:11])[n:12][cH:13]1)[C:14](=[O:15])[OH:16]
CCOC(=O)C(CC)(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1
CCC(CS)(Cc1ccc(N)nc1)C(=O)O
null
null
Cl
Reduction
OtherReaction
df63f36502c6e187beb1211487c3f0937031934a12a3c506c12c51a17b700a31
9a7c4efef36aa8beb2b85c58cd3924b350f3ef529d4eb0778d927167159d9d8b
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].C-C-[O;H0;D2;+0:6]-[C:7](=[O;D1;H0:8])-[C:9]-[C:10]-[S;H0;D2;+0:11]-C(-C)=O>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[O;D1;H0:8]=[C:7](-[OH;D1;+0:6])-[C:9]-[C:10]-[SH;D1;+0:11]
100
[{"value": 100.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylsulfanylmethyl-2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-butyric acid ethyl ester (12.3 mg, 30 μmol) was dissolved in conc. HCl (2 mL) under argon. The solution was heated to reflux for 24 h. Concentration under reduced pressure gave the title compound as the hydrochloride salt (8.3 mg, 100%). Condition...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Ether.Carbo-thioester.Boc
Carboxylic acid.Primary amine.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
null
CCOC(=O)C(CC)(CSC(C)=O)Cc1ccc(NC(=O)OC(C)(C)C)nc1>Cl>CCC(CS)(Cc1ccc(N)nc1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9eb117af31054614bd2029b09386dfab
CC1C(=O)OC(C)(C)OC1=O.Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>Cc1cc(CC2(C)C(=O)OC(C)(C)OC2=O)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
O.C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CBr.CC1(OC(C(C(O1)=O)C)=O)C.C(C)N(CC)CC>>C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CC1(C(OC(OC1=O)(C)C)=O)C
[CH:6]1([CH3:7])[C:8](=[O:9])[O:10][C:11]([CH3:12])([CH3:13])[O:14][C:15]1=[O:16].Br[CH2:5][c:4]1[cH:3][c:2]([CH3:1])[c:19]([N:20]([C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[C:28](=[O:29])[O:30][C:31]([CH3:32])([CH3:33])[CH3:34])[n:18][cH:17]1>>[CH3:1][c:2]1[cH:3][c:4]([CH2:5][C:6]2([CH3:7])[C:8](=[O:9])[...
CC1C(=O)OC(C)(C)OC1=O.Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
Cc1cc(CC2(C)C(=O)OC(C)(C)OC2=O)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
null
null
CS(=O)C
C-C Coupling
OtherReaction
58c01b66b8fc3a6ba5c7ea5eb9ff9622f5543ddf5dc16015d0c2c6736b592a81
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
O=C1OCOC(=O)C1Cc1cccnc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C;D1;H3:7]-[CH;D3;+0:8]1-[C:9](=[O;D1;H0:10])-[#8:11]-[C:12]-[#8:13]-[C:14]-1=[O;D1;H0:15]>>[C;D1;H3:7]-[C;H0;D4;+0:8]1(-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:9](=[O;D1;H0:10])-[#8:11]-[C:12]-[#8:13]-[C:14]-1=[O;D1;H0:15]
107.6
[{"value": 107.6, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CC1(C(OC(OC1=O)(C)C)=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
2-[N,N-bis(tert-Butoxycarbonyl)amino]-5-bromomethyl-3-methyl-pyridin (1.6 g, 4.0 mmol) was added to a solution of 2,2,5-trimethyl-1,3-dioxane-4,6-dione (630 mg, 4.0 mmol) and triethylamine (0.58 mL, 4.2 mmol) in dimethyl sulfoxide (40 mL). The reaction mixture was stirred overnight and water (100 mL) was added. The mix...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
C1COCOC1
C1COCOC1
c1ccncc1.C1COCOC1
HBr
CS(=O)C
null
8
CC1C(=O)OC(C)(C)OC1=O.Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>CS(=O)C>Cc1cc(CC2(C)C(=O)OC(C)(C)OC2=O)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-959be78dd6ce41cfb97af2d09627fb54
Cc1cc(CC2(C)C(=O)OC(C)(C)OC2=O)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>CCOC(=O)C(C)(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
[Na].C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CC1(C(OC(OC1=O)(C)C)=O)C.C(Cl)Cl>>C(C)OC(C(C(=O)O)(C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
CC1([CH3:1])[O:3][C:4](=[O:5])[C:6]([CH3:7])([CH2:8][c:9]2[cH:10][n:11][c:12]([N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[C:21](=[O:22])[O:23][C:24]([CH3:25])([CH3:26])[CH3:27])[c:28]([CH3:29])[cH:30]2)[C:31](=[O:32])[O:33]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH2:8][c:9]1[cH:10][n:11][...
Cc1cc(CC2(C)C(=O)OC(C)(C)OC2=O)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
CCOC(=O)C(C)(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
null
null
C(C)O
Miscellaneous
OtherReaction
63ad813d1b77dce0fe5208aa14f611372b0920cdb45ff078385c4a27a0c20f9d
aec9bcb7276f5cbf55cd2b59ffe4fcb8e927c2173953b25a21ea57417487cdf3
c1ccncc1
C-C1(-[CH3;D1;+0:1])-[O;H0;D2;+0:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6](=[O;D1;H0:7])-[O;H0;D2;+0:8]-1>>[CH3;D1;+0:1]-[C:9]-[O;H0;D2;+0:8]-[C:6](=[O;D1;H0:7])-[C:5]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:2]
101.8
[{"value": 101.8, "product": "C(C)OC(C(C(=O)O)(C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
60
MINUTE
A solution of sodium metal (184 mg, 8.0 mmol) in ethanol (20 mL) was added to a solution of crude 2-[N,N-bis(tert-butoxycarbonyl)amino]-3-methyl-5-(2,2,5-trimethyl-4,6-dioxo-[1,3]dioxan-5-ylmethyl)-pyridin (2.06 g, ˜4.0 mmol) in ethanol (20 mL) under argon. The reaction was stirred for 60 min. and methylene chloride wa...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Carboxylic acid.Ester
C1COCOC1
null
c1ccncc1
Other
C(C)O
null
1
Cc1cc(CC2(C)C(=O)OC(C)(C)OC2=O)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>C(C)O>CCOC(=O)C(C)(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b2cf4b90866342179f06cdfb89ca06a9
CCOC(=O)C(C)(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O>>CCOC(=O)C(C)(CO)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
[BH4-].[Na+].ClC(=O)OC.C(C)OC(C(C(=O)O)(C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O.CCN(CC)CC.Cl>>C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CO)=O
O=[C:8]([C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH2:10][c:11]1[cH:12][n:13][c:14]([N:15]([C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[C:23](=[O:24])[O:25][C:26]([CH3:27])([CH3:28])[CH3:29])[c:30]([CH3:31])[cH:32]1)[OH:9]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH2:8][OH:9])[CH2:10][c:11]1[...
CCOC(=O)C(C)(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
CCOC(=O)C(C)(CO)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
null
null
C(Cl)Cl.C1CCOC1
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
c1ccncc1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[C:3](-[C:4])(-[C;D1;H3:5])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9]>>[C:4]-[C:3](-[C;D1;H3:5])(-[CH2;D2;+0:1]-[O;D1;H1:2])-[C:6](=[O;D1;H0:7])-[#8:8]-[C:9]
49
[{"value": 49.0, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CO)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 48.0, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CO)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
50
MINUTE
Methyl chloroformate (338 μL, 4.4 mmol) was added dropwise to a solution of crude 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-yl methyl)-2-methyl-malonic acid monoethyl ester (1.9 g) and Et3N (641 μL, 4.6 mmol) in THF (30 mL) at −20° C. The reaction mixture was stirred for 50 min., filtered and added dr...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
c1ccncc1
Other
C(Cl)Cl.C1CCOC1
null
0.833333
CCOC(=O)C(C)(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O>C(Cl)Cl.C1CCOC1>CCOC(=O)C(C)(CO)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-aa19bb171de64621a59f5aa38227aad1
CCOC(=O)C(C)(CO)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1.O=C(O)Cc1cccs1>>CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
N(=NC(=O)OC(C)C)C(=O)OC(C)C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.S1C(=CC=C1)CC(=O)O.C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CO)=O>>C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CSC(C)=O)=O
O[CH2:8][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH2:13][c:14]1[cH:15][n:16][c:17]([N:18]([C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[C:26](=[O:27])[O:28][C:29]([CH3:30])([CH3:31])[CH3:32])[c:33]([CH3:34])[cH:35]1.OC([CH2:11][c:10]1ccc[s:9]1)=[O:12]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([...
CCOC(=O)C(C)(CO)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1.O=C(O)Cc1cccs1
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
null
null
C1CCOC1
Protection
OtherReaction
189263d4d19565b9c5c001a81e8abf2a60b1807919ec489920cd4293a1993653
7a83c40990eef465e85ff66652874583517e7c7b69d7750d5f2438fef535f94e
c1ccncc1
O-C(=[O;H0;D1;+0:1])-[CH2;D2;+0:2]-[c;H0;D3;+0:3]1:[s;H0;D2;+0:4]:c:c:c:1.O-[CH2;D2;+0:5]-[C:6](-[C:7])(-[C;D1;H3:8])-[C:9](=[O;D1;H0:10])-[#8:11]-[C:12]>>[C:7]-[C:6](-[C;D1;H3:8])(-[CH2;D2;+0:5]-[S;H0;D2;+0:4]-[C;H0;D3;+0:3](-[CH3;D1;+0:2])=[O;H0;D1;+0:1])-[C:9](=[O;D1;H0:10])-[#8:11]-[C:12]
145.9
[{"value": 145.9, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CSC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Diisopropyl azodicarboxylate (755 μL, 3.91 mmol) was added dropwise to a solution of triphenylphosphine (1.026 g, 3.91 mmol) in THF (10 mL) at 0° C. and the reaction was stirred for 30 min. A solution of thiolacetic acid (279 μL, 3.91 mmol) and 3-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-yl)-2-hydroxyme...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary alcohol
Carbo-thioester
c1ccsc1
null
c1ccncc1
HO-
C1CCOC1
null
0.5
CCOC(=O)C(C)(CO)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1.O=C(O)Cc1cccs1>C1CCOC1>CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0b8e6143433749e2944677c438c6313f
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1>>CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N)c(C)c1
C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)(C)CSC(C)=O)=O>>C(C)OC(C(CC=1C=NC(=C(C1)C)N)(C)CSC(C)=O)=O
CC(C)(C)OC(=O)[N:18](C(=O)OC(C)(C)C)[c:17]1[n:16][cH:15][c:14]([CH2:13][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH2:8][S:9][C:10]([CH3:11])=[O:12])[cH:21][c:19]1[CH3:20]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH2:8][S:9][C:10]([CH3:11])=[O:12])[CH2:13][c:14]1[cH:15][n:16][c:17]([NH2:18])[c:19]([CH3:20...
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N)c(C)c1
null
null
C(=O)(C(F)(F)F)O
Reduction
Boc amine deprotection
f552418eb10f74be275b3d2d2e4940118153e34a0e9e4737d38c7264f73cdda0
c2e7125d1a630bb54d8f171aedbfa925f5104f1c1e5ac8c4ed9643a0c1117a44
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-C(=O)-O-C(-C)(-C)-C)-[c:2](:[c:3]):[#7;a:4]:[c:5]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5]
84
[{"value": 84.0, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N)(C)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.4, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N)(C)CSC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
60
MINUTE
Crude 2-acetylsulfanylmethyl-3-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-yl)-2-methyl-propionic acid ethyl ester (1.46 g) was dissolved in TFA (5 mL) and stirred for 60 min. Concentration under reduced pressure followed by chromathography (toluene/EtOAc, 1:1→1:10→0:1) gave slightly impure 2-acetylsulfan...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carbamic ester.Ether.Ether.Substituted dicarboximide.Boc.Boc
Primary amine
null
null
c1ccncc1
HO-
C(=O)(C(F)(F)F)O
null
1
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1>C(=O)(C(F)(F)F)O>CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N)c(C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b962369971ea4d278e8a5ef08961e63a
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N)c(C)c1>>Cc1cc(CC(C)(CS)C(=O)O)cnc1N
C(C)OC(C(CC=1C=NC(=C(C1)C)N)(C)CSC(C)=O)=O>>NC1=C(C=C(C=N1)CC(C(=O)O)(C)CS)C
CC[O:12][C:10]([C:6]([CH2:5][c:4]1[cH:3][c:2]([CH3:1])[c:15]([NH2:16])[n:14][cH:13]1)([CH3:7])[CH2:8][S:9]C(C)=O)=[O:11]>>[CH3:1][c:2]1[cH:3][c:4]([CH2:5][C:6]([CH3:7])([CH2:8][SH:9])[C:10](=[O:11])[OH:12])[cH:13][n:14][c:15]1[NH2:16]
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N)c(C)c1
Cc1cc(CC(C)(CS)C(=O)O)cnc1N
null
null
Cl
Reduction
OtherReaction
1bcd8cbb2f136b4bcba1690e9ba45c4e43c89ba76f0e22de82a7d3fe318c82a9
5654c46fe4cb226f88ec3c899c7f9be1825c357673ea686958f9ef4883ee1db3
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[S;H0;D2;+0:6]-C(-C)=O>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[C:4]-[C:5]-[SH;D1;+0:6]
96
[{"value": 96.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylsulfanylmethyl-3-(6-amino-5-methyl-pyridin-3-yl)-2-methyl-propionic acid ethyl ester (17 mg, 40 μmol) was dissolved in conc. HCl (2 mL) under argon. The solution was heated to reflux for 150 min. Concentration under reduced pressure gave the title compound as the hydrochloride salt (10.7 mg, 96%). Conditions: S...
10.6084/m9.figshare.5104873.v1
null
Ester.Carbo-thioester
Carboxylic acid.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
null
CCOC(=O)C(C)(CSC(C)=O)Cc1cnc(N)c(C)c1>Cl>Cc1cc(CC(C)(CS)C(=O)O)cnc1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-36d991e903c24644903420e72332da4d
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]O[Si](C)(C)C(C)(C)C.Cc1cc(Br)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>Cc1cc(C(C)(C)O[SiH2]C(C)(C)C)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
[F-].[K+].BrC=1C=C(C(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C.C(C)(C)(C)[Si](OC[Sn](CCCC)(CCCC)CCCC)(C)C.ClCCCl.C(C)OCC>>C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)C(O[SiH2]C(C)(C)C)(C)C
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2:5][O:8][Si:9]([CH3:6])([CH3:7])[C:10]([CH3:11])([CH3:12])[CH3:13].Br[c:4]1[cH:3][c:2]([CH3:1])[c:16]([N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[n:15][cH:14]1>>[CH3:1][c:2]1[cH:3][c:4]([C:5]([CH3:6])([CH3:7]...
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]O[Si](C)(C)C(C)(C)C.Cc1cc(Br)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
Cc1cc(C(C)(C)O[SiH2]C(C)(C)C)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
null
C-C Coupling
OtherReaction
2c35ffcca42587548be5417494593198fc16ef4537fcb3507e56ecb0940f483d
e19d215278fe89455f513eea1f431a9cbd352fd26641180be69d9777a377b4b5
c1ccncc1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1.C-C-C-[CH2]-[Sn](-[CH2;D2;+0:7]-[#8:8]-[Si;H0;D4;+0:9](-[CH3;D1;+0:10])(-[CH3;D1;+0:11])-[C:12](-[C;D1;H3:13])(-[C;D1;H3:14])-[C;D1;H3:15])(-[CH2]-C-C-C)-[CH2]-C-C-C>>[C;D1;H3:13]-[C:12](-[C;D1;H3:14])(-[C;D1;H3:15])-[SiH2;D2;+0:9]-[#8:8]-[C;H0;D4;+0:7](-[CH3;D1;+0:...
59
[{"value": 59.0, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)C(O[SiH2]C(C)(C)C)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
A solution of 5-bromo-2-[N,N-bis(tert-butoxycarbonyl)amino]-3-methyl-pyridin (26.0 g, 67.1 mmol), tert-butyl-dimethyl-tributylstannanylmethoxy-silane (47.6 g, 109 mmol), and bis(triphenylphosphine)palladium(II) dichloride (0.90 g, 1.42 mmol) in 1,2-dichloroethane (80 mL) was stirred at 90° C. for two days. The mixture ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.TMS ether protective group.Tin
null
c1ccncc1
c1ccncc1
c1ccncc1
HBr.Sn
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
0
0.5
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]O[Si](C)(C)C(C)(C)C.Cc1cc(Br)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl>Cc1cc(C(C)(C)O[SiH2]C(C)(C)C)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7f016dac5a71499cab1442bd665fa2a5
Cc1cc(C(C)(C)O[SiH2]C(C)(C)C)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>Cc1cc(CO)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)C(O[SiH2]C(C)(C)C)(C)C>>C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CO
CC(C)(C)[SiH2][O:6][C:5](C)(C)[c:4]1[cH:3][c:2]([CH3:1])[c:9]([N:10]([C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17])[C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[n:8][cH:7]1>>[CH3:1][c:2]1[cH:3][c:4]([CH2:5][OH:6])[cH:7][n:8][c:9]1[N:10]([C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17])[C:18]...
Cc1cc(C(C)(C)O[SiH2]C(C)(C)C)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
Cc1cc(CO)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
null
null
C1CCOC1
Deprotection
OtherReaction
d7487e9652d81f9226fa8fb90bf02725deb1441d4abc97ee4fdbe439e00122e0
ff9889ffd40f59bd281424811967f384d29acb01a2d54e10590c5a677f81d17a
c1ccncc1
C-C(-C)(-C)-[SiH2]-[O;H0;D2;+0:1]-[C;H0;D4;+0:2](-C)(-C)-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
59.4
[{"value": 59.0, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 59.4, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Tetrabutylammonium fluoride (25.1 g 79.6 mmol) was added to a solution of 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-(tert-butyl-dimethyl-silanyloxymethyl)-3-methylpyridin (18.0 g, 39.8 mmol) in THF (150 mL). The reaction mixture was stirred overnight at room temperature. Concentration under reduced pressure followed by f...
10.6084/m9.figshare.5104873.v1
null
null
Primary alcohol
null
null
c1ccncc1
Other
C1CCOC1
null
8
Cc1cc(C(C)(C)O[SiH2]C(C)(C)C)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>C1CCOC1>Cc1cc(CO)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-56843a12b02b48b19d22edc5fd10549e
BrC(Br)(Br)Br.Cc1cc(CO)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(Br)(Br)(Br)Br.C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CO>>BrCC=1C=C(C(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C
BrC(Br)(Br)[Br:6].O[CH2:5][c:4]1[cH:3][c:2]([CH3:1])[c:9]([N:10]([C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17])[C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[n:8][cH:7]1>>[CH3:1][c:2]1[cH:3][c:4]([CH2:5][Br:6])[cH:7][n:8][c:9]1[N:10]([C:11](=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[CH3:17])[C:18](=[O...
BrC(Br)(Br)Br.Cc1cc(CO)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
null
null
ClCCl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
c1ccncc1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
84.5
[{"value": 77.0, "product": "BrCC=1C=C(C(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.5, "product": "BrCC=1C=C(C(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Triphenylphosphine (7.43 g, 28.3 mmol) and CBr4 (9.49 g, 28.6 mmol) was added to a solution of 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-hydroxymethyl-3-methylpyridin (8.00 g, 23.6 mmol) in dichloromethane (220 mL) at 0° C. The reaction mixture was stirred for 3 h and was then concentrated under reduced pressure. Flash c...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccncc1
HBr
ClCCl
null
3
BrC(Br)(Br)Br.Cc1cc(CO)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>ClCCl>Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bae3f117e03c4bedae6115f447a87479
CCOC(=O)CC(=O)OCC.Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
C(C)(=O)OCC.C(CC(=O)OCC)(=O)OCC.[H-].[Na+].C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C=C1C)CBr>>C(C)OC(C(C(=O)OCC)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:30](=[O:31])[O:32][CH2:33][CH3:34].Br[CH2:7][c:8]1[cH:9][n:10][c:11]([N:12]([C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[c:27]([CH3:28])[cH:29]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][n:10]...
CCOC(=O)CC(=O)OCC.Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
null
null
CN(C)C=O
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
c1ccncc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
50
[{"value": 50.0, "product": "C(C)OC(C(C(=O)OCC)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 49.9, "product": "C(C)OC(C(C(=O)OCC)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a suspension of NaH (0.24 g, 6.0 mmol, 60%) in DMF (5 mL) was added diethyl malonate (0.91 mL, 6.0 mmol) and the mixture was stirred for 15 min. A solution 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-bromomethyl-3-methyl-pyridin (2.0 g, 5.0 mmol) in DMF (5 mL) was added and the resulting solution stirred for 120 min at ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccncc1
HBr
CN(C)C=O
null
0.25
CCOC(=O)CC(=O)OCC.Cc1cc(CBr)cnc1N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C>CN(C)C=O>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e3ec7f046bc24f2f8fdc07ad0f018346
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC>>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
[OH-].[K+].C(C)OC(C(C(=O)OCC)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O>>C(C)OC(C(C(=O)O)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
CC[O:32][C:30]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][c:8]1[cH:9][n:10][c:11]([N:12]([C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[c:27]([CH3:28])[cH:29]1)=[O:31]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][n:10][c:11]([N:12]([C...
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
null
null
C(Cl)Cl.C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
88.4
[{"value": 88.0, "product": "C(C)OC(C(C(=O)O)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.4, "product": "C(C)OC(C(C(=O)O)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of KOH (154 mg, 2.75 mmol) in ethanol (2 mL) was added to a solution 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-ylmethyl)-malonic acid diethyl ester (1.2 g, 2.50 mmol) in ethanol (10 mL) and methylene chloride (4 mL) at 0° C. The mixture was stirred for 18 h at room temperature. The mixture ...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1
Other
C(Cl)Cl.C(C)O
null
18
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC>C(Cl)Cl.C(C)O>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f93ca83672634c3ca17565cf8c3f0b67
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O>>C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
C(C)NCC.C(C)OC(C(C(=O)O)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O.C=O.C(C)(=O)OCC>>C(C)OC(C(=C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
O=[C:1](O)[CH:2]([CH2:3][c:4]1[cH:5][n:6][c:7]([N:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[c:23]([CH3:24])[cH:25]1)[C:26](=[O:27])[O:28][CH2:29][CH3:30]>>[CH2:1]=[C:2]([CH2:3][c:4]1[cH:5][n:6][c:7]([N:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:...
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
485594ce7bba157615ffbb01ccede84a4e638576571b5d04649a06f3d4b7bce0
55e5b5078322f9f4fb0a7e9b5fc8a8cb9084e9135b447b8c441ad0800765792e
c1ccncc1
O-[C;H0;D3;+0:1](=O)-[CH;D3;+0:2](-[C:3]-[c:4]:[c:5]:[#7;a:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]>>[#7;a:6]:[c:5]:[c:4]-[C:3]-[C;H0;D3;+0:2](=[CH2;D1;+0:1])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]
73.5
[{"value": 73.0, "product": "C(C)OC(C(=C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 73.5, "product": "C(C)OC(C(=C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Diethylamine (0.26 g, 2.67 mmol) was added a mixture of 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-ylmethyl)-malonic acid monoethyl ester (1.0 g, 2.2 mmol) and 37% aq. solution of formaldehyde (0.24 g, 3.00 mmol) in methylene chloride (2 mL) at 0° C. The mixture was stirred for 16 h at room temperature...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester.Vinyl
null
null
c1ccncc1
Other
C(Cl)Cl
null
16
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)O>C(Cl)Cl>C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3a1653c40d78486e965a2443fb236cdc
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC.CC(O)=S>>CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
C(C)N(CC)CC.C(C)OC(C(=C)CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O.C(C)(=S)O.C(C)(=O)OCC>>C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[CH2:7])[CH2:12][c:13]1[cH:14][n:15][c:16]([N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:32]([CH3:33])[cH:34]1.[S:8]=[C:9]([CH3:10])[OH:11]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10...
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC.CC(O)=S
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
null
null
null
Protection
OtherReaction
56aa090d67fbecbea8a1963579cc34949775a09653b2b2f2795c609c60e70c77
5a9b0d631147b21b844b3c73866d1d81ab543538a176ebae28118ae7e39e572f
c1ccncc1
[#7;a:1]:[c:2]:[c:3]-[C:4]-[C;H0;D3;+0:5](=[CH2;D1;+0:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10].[C;D1;H3:11]-[C;H0;D3;+0:12](-[OH;D1;+0:13])=[S;H0;D1;+0:14]>>[#7;a:1]:[c:2]:[c:3]-[C:4]-[CH;D3;+0:5](-[CH2;D2;+0:6]-[S;H0;D2;+0:14]-[C;H0;D3;+0:12](-[C;D1;H3:11])=[O;H0;D1;+0:13])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]
43
[{"value": 43.0, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Triethylamine (0.234 mL, 1.68 mmol) was added to a solution of 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-ylmethyl)-acrylic acid ethyl ester (0.68 g, 1.61 mmol) in thioacetic acid (3 mL) at 0° C. The mixture was stirred at room temperature for 16 h. Ethyl acetate was added and the organic phase was was...
10.6084/m9.figshare.5104873.v1
null
Ester.Thiocarbonyl.Vinyl
Ester.Carbo-thioester
null
null
c1ccncc1
null
null
null
16
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1)C(=O)OCC.CC(O)=S>>CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-03fea22a728046a797595b16b44adb1c
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1>>Cc1cc(CC(CS)C(=O)O)cnc1N
C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O>>NC1=C(C=C(C=N1)CC(C(=O)O)CS)C
CC[O:11][C:9]([CH:6]([CH2:5][c:4]1[cH:3][c:2]([CH3:1])[c:14]([N:15](C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)[n:13][cH:12]1)[CH2:7][S:8]C(C)=O)=[O:10]>>[CH3:1][c:2]1[cH:3][c:4]([CH2:5][CH:6]([CH2:7][SH:8])[C:9](=[O:10])[OH:11])[cH:12][n:13][c:14]1[NH2:15]
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1
Cc1cc(CC(CS)C(=O)O)cnc1N
null
null
Cl
Reduction
OtherReaction
ff200d63748925ecb928aee95d999f108474ef3634c58d22fe1e9be9ac805fa3
430680ed2de5eb87de586bf5706158a5dd503c4be3ff91566980452c5549779b
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-C(=O)-O-C(-C)(-C)-C)-[c:2](:[c:3]):[#7;a:4]:[c:5].C-C-[O;H0;D2;+0:6]-[C:7](=[O;D1;H0:8])-[C:9]-[C:10]-[S;H0;D2;+0:11]-C(-C)=O>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[O;D1;H0:8]=[C:7](-[OH;D1;+0:6])-[C:9]-[C:10]-[SH;D1;+0:11]
115.7
[{"value": 100.0, "product": "NC1=C(C=C(C=N1)CC(C(=O)O)CS)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 115.7, "product": "NC1=C(C=C(C=N1)CC(C(=O)O)CS)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylsulfanylmethyl-3-(6-[N,N-bis(tert-butoxycarbonyl)amino]-5-methyl-pyridin-3-yl)-propionic acid ethyl ester (17 mg, 0.034 mmol) was dissolved in conc. HCl (3.0 mL). The solution was heated to reflux for 1 h. Concentration under reduced pressure gave the title compound (8.9 mg, 100%) as the hydrochloride salt. Con...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carbamic ester.Ester.Ether.Ether.Substituted dicarboximide.Carbo-thioester.Boc.Boc
Carboxylic acid.Primary amine.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
null
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1>Cl>Cc1cc(CC(CS)C(=O)O)cnc1N
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9c5095105cfe4857aa00178cf8638848
Br.Cc1ccnc(N)c1>>Cc1cc(N)ncc1Br
NC1=NC=CC(=C1)C.Br.OO.C([O-])([O-])=O.[Na+].[Na+]>>NC1=NC=C(C(=C1)C)Br
[BrH:9].[CH3:1][c:2]1[cH:3][c:4]([NH2:5])[n:6][cH:7][cH:8]1>>[CH3:1][c:2]1[cH:3][c:4]([NH2:5])[n:6][cH:7][c:8]1[Br:9]
Br.Cc1ccnc(N)c1
Cc1cc(N)ncc1Br
null
null
null
Functional Group Addition
Bromination
7c108e53aa6849672ac0ea1998cfd24df7835b0d1bc5738d16f4d561a472c88e
0a2f22058f27970cef4a98a778644dbe9c44e91f66c74cd24db321993177608a
c1ccncc1
[BrH;D0;+0:1].[C;D1;H3:2]-[c:3]1:[c:4]:[c:5]:[#7;a:6]:[c:7]:[cH;D2;+0:8]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:8]1:[c:7]:[#7;a:6]:[c:5]:[c:4]:[c:3]:1-[C;D1;H3:2]
40
[{"value": 40.0, "product": "NC1=NC=C(C(=C1)C)Br", "details": "PERCENTYIELD", "is_desired": false}]
70
CELSIUS
90
MINUTE
2-Amino-4-methylpyridine (110 g, 1.02 mol) in hydrobromic acid (1 L, 48%) was stirred at 70° C. and a solution of hydrogen peroxide (300 mL, 15%) was added dropwise over a one h at such a rate that the temperature of the reaction mixture remained at 70-80° C. The mixture was stirred for 90 min at 70° C. and poured onto...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccncc1
c1ccncc1
c1ccncc1
null
null
70
1.5
Br.Cc1ccnc(N)c1>>Cc1cc(N)ncc1Br
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-11b564af92244385904b20e883187645
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]O[Si](C)(C)C(C)(C)C.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1Br>>Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1C(C)(C)O[SiH2]C(C)(C)C
[F-].[K+].C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)Br.C(C)(C)(C)[Si](OC[Sn](CCCC)(CCCC)CCCC)(C)C.ClCCCl.C(C)OCC>>C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)C(O[SiH2]C(C)(C)C)(C)C
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2:23][O:26][Si:27]([CH3:24])([CH3:25])[C:28]([CH3:29])([CH3:30])[CH3:31].Br[c:22]1[c:2]([CH3:1])[cH:3][c:4]([N:5]([C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([N:5]([C:6](=[O:7])[O:...
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]O[Si](C)(C)C(C)(C)C.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1Br
Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1C(C)(C)O[SiH2]C(C)(C)C
null
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
null
C-C Coupling
OtherReaction
2c35ffcca42587548be5417494593198fc16ef4537fcb3507e56ecb0940f483d
e19d215278fe89455f513eea1f431a9cbd352fd26641180be69d9777a377b4b5
c1ccncc1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[c:5]:[c:6]:1-[C;D1;H3:7].C-C-C-[CH2]-[Sn](-[CH2;D2;+0:8]-[#8:9]-[Si;H0;D4;+0:10](-[CH3;D1;+0:11])(-[CH3;D1;+0:12])-[C:13](-[C;D1;H3:14])(-[C;D1;H3:15])-[C;D1;H3:16])(-[CH2]-C-C-C)-[CH2]-C-C-C>>[C;D1;H3:7]-[c:6]1:[c:5]:[c:4]:[#7;a:3]:[c:2]:[c;H0;D3;+0:1]:1-[C;H0;D4;+0:8](-[CH3;D1...
57
[{"value": 57.0, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)C(O[SiH2]C(C)(C)C)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
A solution of 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-bromo-4-methylpyridin (15.0 g, 38.70 mmol), tert-butyl-dimethyl-tributylstannanylmethoxy-silane (25.4 g, 58.3 mmol), and bis(triphenylphosphine)palladium(II) dichloride (0.90 g, 1.42 mmol) in 1,2dichloroethane (50 mL) was stirred at 90° C. for two days. The mixture ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.TMS ether protective group.Tin
null
c1ccncc1
c1ccncc1
c1ccncc1
HBr.Sn
Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl
0
0.5
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[CH2]O[Si](C)(C)C(C)(C)C.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1Br>Cl[Pd]([P](C1=CC=CC=C1)(C2=CC=CC=C2)C3=CC=CC=C3)([P](C4=CC=CC=C4)(C5=CC=CC=C5)C6=CC=CC=C6)Cl>Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1C(C)(C)O[SiH2]C(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5665354fd2f7409e9a81995370c974a7
Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1C(C)(C)O[SiH2]C(C)(C)C>>Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CO
[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)C(O[SiH2]C(C)(C)C)(C)C>>C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)CO
CC(C)(C)[SiH2][O:24][C:23](C)(C)[c:22]1[c:2]([CH3:1])[cH:3][c:4]([N:5]([C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([N:5]([C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3...
Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1C(C)(C)O[SiH2]C(C)(C)C
Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CO
null
null
C1CCOC1
Deprotection
OtherReaction
d7487e9652d81f9226fa8fb90bf02725deb1441d4abc97ee4fdbe439e00122e0
ff9889ffd40f59bd281424811967f384d29acb01a2d54e10590c5a677f81d17a
c1ccncc1
C-C(-C)(-C)-[SiH2]-[O;H0;D2;+0:1]-[C;H0;D4;+0:2](-C)(-C)-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
67
[{"value": 67.0, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)CO", "details": "PERCENTYIELD", "is_desired": false}, {"value": 60.8, "product": "C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)CO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Tetrabutylammonium fluoride (13.9 g, 44.1 mmol) was added to a solution of 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-(tert-butyl-dimethyl-silanyloxymethyl)-4-methylpyridin (10.0 g, 24.3 mmol) in THF (100 mL). The reaction mixture was stirred for 3 h at room temperature. Concentration under reduced pressure followed by fl...
10.6084/m9.figshare.5104873.v1
null
null
Primary alcohol
null
null
c1ccncc1
Other
C1CCOC1
null
3
Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1C(C)(C)O[SiH2]C(C)(C)C>C1CCOC1>Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CO
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eb5aa5ebdc914155b2566bb3679d71a8
BrC(Br)(Br)Br.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CO>>Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CBr
C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C(Br)(Br)(Br)Br.C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)CO>>BrCC=1C(=CC(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C
BrC(Br)(Br)[Br:24].O[CH2:23][c:22]1[c:2]([CH3:1])[cH:3][c:4]([N:5]([C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([N:5]([C:6](=[O:7])[O:8][C:9]([CH3:10])([CH3:11])[CH3:12])[C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18]...
BrC(Br)(Br)Br.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CO
Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CBr
null
null
ClCCl
Functional Group Interconversion
Appel reaction
752e1807cd47d8316010cc3f92eab16c5a89ffb844d9514fcae469ba993c78dd
2c6b51fb1e17cb2c93d565e0423c75825df2c8e11c870e0c98b278f20ba9f3ad
c1ccncc1
Br-C(-Br)(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
90.1
[{"value": 90.0, "product": "BrCC=1C(=CC(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.1, "product": "BrCC=1C(=CC(=NC1)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Triphenylphosphine (4.69 g, 17.9 mmol) and CBr4 (4.89 g, 14.8 mmol) was added to a solution of 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-hydroxymethyl-4-methylpyridin (5.00 g, 22.0 mmol) in dichloromethane (130 mL) at 0° C. The reaction mixture was stirred for 3 h and was then diluted with dichloromethane. The organic ph...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Tertiary halide.Primary alcohol
Primary halide
null
null
c1ccncc1
HBr
ClCCl
null
3
BrC(Br)(Br)Br.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CO>ClCCl>Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CBr
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-67ff9859d3e345c2ae19712d6f3b494f
CCOC(=O)CC(=O)OCC.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CBr>>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
C(C)(=O)OCC.C(CC(=O)OCC)(=O)OCC.[H-].[Na+].C(C)(C)(C)OC(=O)N(C(=O)OC(C)(C)C)C1=NC=C(C(=C1)C)CBr>>C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:30](=[O:31])[O:32][CH2:33][CH3:34].Br[CH2:7][c:8]1[cH:9][n:10][c:11]([N:12]([C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[cH:27][c:28]1[CH3:29]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][n:10][c...
CCOC(=O)CC(=O)OCC.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CBr
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
null
null
CN(C)C=O
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
c1ccncc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
48
[{"value": 48.0, "product": "C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 47.9, "product": "C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a suspension of NaH (0.24 g, 6.0 mmol, 60%) in DMF (5 mL) was added diethyl malonate (0.91 mL, 6.0 mmol) and the mixture was stirred for 15 min. A solution 2-[N,N-bis(tert-butoxycarbonyl)amino]-5-bromomethyl-4-methyl-pyridin (2.0 g, 5.0 mmol) in DMF (5 mL) was added and the resulting solution stirred for 120 min at ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccncc1
HBr
CN(C)C=O
null
0.25
CCOC(=O)CC(=O)OCC.Cc1cc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)ncc1CBr>CN(C)C=O>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b84a505c29024323a7f7daa2e2f9b332
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC>>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)O
[OH-].[K+].C(C)OC(C(C(=O)OCC)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O>>C(C)OC(C(C(=O)O)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
CC[O:32][C:30]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][c:8]1[cH:9][n:10][c:11]([N:12]([C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[C:20](=[O:21])[O:22][C:23]([CH3:24])([CH3:25])[CH3:26])[cH:27][c:28]1[CH3:29])=[O:31]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][c:8]1[cH:9][n:10][c:11]([N:12]([C:1...
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)O
null
null
C(Cl)Cl.C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
97
[{"value": 97.0, "product": "C(C)OC(C(C(=O)O)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.5, "product": "C(C)OC(C(C(=O)O)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of KOH (141 mg, 2.52 mmol) in ethanol (2 mL) was added to a solution 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]4-methyl-pyridin-3-ylmethyl)-malonic acid diethyl ester (1.1 g, 2.29 mmol) in ethanol (10 mL) and methylene chloride (4 mL) at 0° C. The mixture was stirred for 18 h at room temperature. The mixture w...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1
Other
C(Cl)Cl.C(C)O
null
18
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC>C(Cl)Cl.C(C)O>CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-bfa4f575661a4f058260736ab655e8f3
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)O>>C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
C(C)NCC.C(C)OC(C(C(=O)O)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O.C=O.C(C)(=O)OCC>>C(C)OC(C(=C)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O
O=[C:1](O)[CH:2]([CH2:3][c:4]1[cH:5][n:6][c:7]([N:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14])[CH3:15])[C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[cH:23][c:24]1[CH3:25])[C:26](=[O:27])[O:28][CH2:29][CH3:30]>>[CH2:1]=[C:2]([CH2:3][c:4]1[cH:5][n:6][c:7]([N:8]([C:9](=[O:10])[O:11][C:12]([CH3:13])([CH3:14...
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)O
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
485594ce7bba157615ffbb01ccede84a4e638576571b5d04649a06f3d4b7bce0
55e5b5078322f9f4fb0a7e9b5fc8a8cb9084e9135b447b8c441ad0800765792e
c1ccncc1
O-[C;H0;D3;+0:1](=O)-[CH;D3;+0:2](-[C:3]-[c:4]:[c:5]:[#7;a:6])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]>>[#7;a:6]:[c:5]:[c:4]-[C:3]-[C;H0;D3;+0:2](=[CH2;D1;+0:1])-[C:7](=[O;D1;H0:8])-[#8:9]-[C:10]
88
[{"value": 88.0, "product": "C(C)OC(C(=C)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 87.6, "product": "C(C)OC(C(=C)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Diethylamine (0.26 g, 2.67 mmol) was added a mixture of 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]-4-methyl-pyridin-3-ylmethyl)-malonic acid monoethyl ester (1.0 g, 2.2 mmol) and 37% aq. solution of formaldehyde (0.24 g, 3.00 mmol) in methylene chloride (2 mL) at 0° C. The mixture was stirred for 16 h at room temperature...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester.Vinyl
null
null
c1ccncc1
Other
C(Cl)Cl
null
16
CCOC(=O)C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)O>C(Cl)Cl>C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-85be6c3d5cf947ad8578ebfa34a63d26
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC.CC(O)=S.CCN(CC)CC.CCOC(C)=O>>CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1.CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C
C(C)N(CC)CC.C(C)OC(C(=C)CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)=O.C(C)(=S)O.C(C)(=O)OCC>>C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O.C(C)OC(C(CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O
[CH3:18][C:21]([O:20][C:59](=[O:19])[N:51]([C:25](=[O:26])[O:27][C:28]([CH3:29])([CH3:30])[CH3:31])[c:50]1[n:49][cH:48][c:47]([CH2:46][C:40]([C:38]([O:37][CH2:36][CH3:35])=[O:39])=[CH2:41])[c:67]([CH3:68])[cH:66]1)([CH3:58])[CH3:65].[S:8]=[C:9]([CH3:10])[OH:11].[CH3:7][CH2:12][N:15]([CH2:14][CH3:13])[CH2:16][CH3:32].[C...
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC.CC(O)=S.CCN(CC)CC.CCOC(C)=O
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1.CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C
null
null
null
Aromatic Heterocycle Formation
OtherReaction
032ef00a7acaabf6ca8902421766a9be71716253a44363dc16930c2ebd884199
02573f00161c0a40ac11ef724be710e73cabd6145119dfbb27fe4f0b665bb2a6
c1ccncc1.c1ccncc1
[C;D1;H3:1]-[C;H0;D3;+0:2](-[OH;D1;+0:3])=[S;H0;D1;+0:4].[CH3;D1;+0:5]-[CH2;D2;+0:6]-[N;H0;D3;+0:7](-[CH2;D2;+0:8]-[CH3;D1;+0:9])-[CH2;D2;+0:10]-[CH3;D1;+0:11].[C:12]-[#8:13]-[C:14](-[CH3;D1;+0:15])=[O;D1;H0:16].[C:17]-[#8:18]-[C:19](=[O;D1;H0:20])-[C;H0;D3;+0:21](=[CH2;D1;+0:22])-[C:23]-[c:24]:[c:25]:[#7;a:26]:[c:27](...
21
[{"value": 21.0, "product": "C(C)OC(C(CC=1C=NC(=C(C1)C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
Triethylamine (0.279 mL, 2.0 mmol) was added to a solution of 2-(6-[N,N-bis(tert-butoxycarbonyl)amino]-4-methyl-pyridin-3-ylmethyl)-acrylic acid ethyl ester (0.8 g, 1.9 mmol) in thioacetic acid (3 mL) at 0° C. The mixture was stirred at room temperature for 16 h. Ethyl acetate was added and the organic phase was washed...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carbamic ester.Ester.Ester.Ether.Ether.Substituted dicarboximide.Tertiary amine.Thiocarbonyl.Vinyl.Boc.Boc
Carbamic ester.Carbamic ester.Carbamic ester.Carbamic ester.Ester.Ester.Ether.Ether.Ether.Ether.Substituted dicarboximide.Substituted dicarboximide.Carbo-thioester.Carbo-thioester.Boc.Boc.Boc.Boc
null
c1ccncc1
c1ccncc1.c1ccncc1
Other
null
null
16
C=C(Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C)C(=O)OCC.CC(O)=S.CCN(CC)CC.CCOC(C)=O>>CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)c(C)c1.CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d41aba1fce454adcb3f51d2dde176afd
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C>>Cc1cc(N)ncc1CC(CS)C(=O)O
C(C)OC(C(CC=1C=NC(=CC1C)N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)CSC(C)=O)=O>>NC1=CC(=C(C=N1)CC(C(=O)O)CS)C
CC[O:15][C:13]([CH:10]([CH2:9][c:8]1[c:2]([CH3:1])[cH:3][c:4]([N:5](C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)[n:6][cH:7]1)[CH2:11][S:12]C(C)=O)=[O:14]>>[CH3:1][c:2]1[cH:3][c:4]([NH2:5])[n:6][cH:7][c:8]1[CH2:9][CH:10]([CH2:11][SH:12])[C:13](=[O:14])[OH:15]
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C
Cc1cc(N)ncc1CC(CS)C(=O)O
null
null
Cl
Reduction
OtherReaction
ff200d63748925ecb928aee95d999f108474ef3634c58d22fe1e9be9ac805fa3
430680ed2de5eb87de586bf5706158a5dd503c4be3ff91566980452c5549779b
c1ccncc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-C(=O)-O-C(-C)(-C)-C)-[c:2](:[c:3]):[#7;a:4]:[c:5].C-C-[O;H0;D2;+0:6]-[C:7](=[O;D1;H0:8])-[C:9]-[C:10]-[S;H0;D2;+0:11]-C(-C)=O>>[NH2;D1;+0:1]-[c:2](:[c:3]):[#7;a:4]:[c:5].[O;D1;H0:8]=[C:7](-[OH;D1;+0:6])-[C:9]-[C:10]-[SH;D1;+0:11]
114.8
[{"value": 98.0, "product": "NC1=CC(=C(C=N1)CC(C(=O)O)CS)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 114.8, "product": "NC1=CC(=C(C=N1)CC(C(=O)O)CS)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
2-Acetylsulfanylmethyl-3-(6-[N,N-bis(tert-butoxycarbonyl)amino]-4-methyl-pyridin-3-yl)-propionic acid ethyl ester (36 mg, 0.072 mmol) was dissolved in conc. HCl (3.0 mL). The solution was heated to reflux for 1 h. Concentration under reduced pressure gave the title compound (18.7 mg, 98%) as the hydrochloride salt. Con...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Carbamic ester.Ester.Ether.Ether.Substituted dicarboximide.Carbo-thioester.Boc.Boc
Carboxylic acid.Primary amine.Aliphatic thiol
null
null
c1ccncc1
HO-
Cl
null
null
CCOC(=O)C(CSC(C)=O)Cc1cnc(N(C(=O)OC(C)(C)C)C(=O)OC(C)(C)C)cc1C>Cl>Cc1cc(N)ncc1CC(CS)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1d62ca02886d475b84f45385af6939a4
CC(C)(C)OC(=O)N1CCC(CO)CC1>>CC(C)(C)OC(=O)N1CCC(C=O)CC1
C(C)(C)(C)OC(=O)N1CCC(CC1)CO.C(C)OCC>>C(C)(C)(C)OC(=O)N1CCC(CC1)C=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][OH:13])[CH2:14][CH2:15]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH:12]=[O:13])[CH2:14][CH2:15]1
CC(C)(C)OC(=O)N1CCC(CO)CC1
CC(C)(C)OC(=O)N1CCC(C=O)CC1
null
null
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
C1CCNCC1
[C:1]-[C:2](-[CH2;D2;+0:3]-[OH;D1;+0:4])-[C:5]>>[C:1]-[C:2](-[CH;D2;+0:3]=[O;H0;D1;+0:4])-[C:5]
81.7
[{"value": 81.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 81.7, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
90
MINUTE
Periodinane (26.9 g, 63.5 mmol) was added to a solution of 1-tert-butoxycarbonyl-piperidine-4-methanol (10.5 g, 48.8 mmol) in methylene chloride (200 mL) and the mixture was stirred for 90 min. Diethyl ether was added and precipitates were removed by extraction with 10% Na2S2O3/saturated NaHCO3 (1:1, 300 mL). The organ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
C1CC[NH]CC1
null
C(Cl)Cl
null
1.5
CC(C)(C)OC(=O)N1CCC(CO)CC1>C(Cl)Cl>CC(C)(C)OC(=O)N1CCC(C=O)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a05c56976b414edf8d5d8980bc7e38dc
CC(C)(C)OC(=O)N1CCC(C=O)CC1.CCOC(=O)CC(=O)OCC>>CCOC(=O)C(=CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OCC
C(CC(=O)OCC)(=O)OCC.C(C)(C)(C)OC(=O)N1CCC(CC1)C=O.N1CCCCC1.C(C)(=O)O>>C(C)OC(C(C(=O)OCC)=CC1CCN(CC1)C(=O)OC(C)(C)C)=O
O=[CH:7][CH:8]1[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:19][CH2:20]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:21](=[O:22])[O:23][CH2:24][CH3:25]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[CH:7][CH:8]1[CH2:9][CH2:10][N:11]([C:12](=[O:13])[O:14][C:15]([CH3:16])([CH3:17])[CH3:18])[...
CC(C)(C)OC(=O)N1CCC(C=O)CC1.CCOC(=O)CC(=O)OCC
CCOC(=O)C(=CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OCC
null
null
C(Cl)Cl.CCOC(=O)C
C-C Coupling
Aldol condensation
4308c3bc8a698ffc0b4a25652616c227140ef668f7c572096e661e9937e780ad
fae8d7810715ce1cb0ea563a010deed21a5c5db9b9f45a5f7ae1c022defa3e22
C1CCNCC1
O=[CH;D2;+0:1]-[C:2](-[C:3])-[C:4].[C:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[CH2;D2;+0:9]-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]>>[C:3]-[C:2](-[CH;D2;+0:1]=[C;H0;D3;+0:9](-[C:7](=[O;D1;H0:8])-[#8:6]-[C:5])-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13])-[C:4]
41.3
[{"value": 40.0, "product": "C(C)OC(C(C(=O)OCC)=CC1CCN(CC1)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 41.3, "product": "C(C)OC(C(C(=O)OCC)=CC1CCN(CC1)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
72
HOUR
To a solution of diethyl malonate (710 μL, 4.7 mmol) and 4-formyl-piperidine-1-carboxylic acid tert-butyl ester (1.0 g,4.7 mmol) in methylene chloride (5 mL) was added piperidine (46 μL, 0.47 mmol) and acetic acid (27 μL, 0.47 mmol). The reaction mixture was stirred for 72 h at room temperature and then for 16 h at 45°...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester.Ester
Ester.Ester
null
null
C1CC[NH]CC1
HO-
C(Cl)Cl.CCOC(=O)C
null
72
CC(C)(C)OC(=O)N1CCC(C=O)CC1.CCOC(=O)CC(=O)OCC>C(Cl)Cl.CCOC(=O)C>CCOC(=O)C(=CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1dc4c076a3904857b216076645d79004
CCOC(=O)C(=CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OCC>>CCOC(=O)C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
[Li]C.C(C)OC(C(C(=O)OCC)=CC1CCN(CC1)C(=O)OC(C)(C)C)=O.[NH4+].[OH-]>>C(C)OC(C(C(=O)OCC)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([C:7](=[O:8])[O:9][CH2:10][CH3:11])=[CH:12][CH:14]1[CH2:15][CH2:16][N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([C:7](=[O:8])[O:9][CH2:10][CH3:11])[CH:12]([CH3:13])[CH:14]1[CH2:15][CH2:16][N:17]([C:18](=[O:...
CCOC(=O)C(=CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OCC
CCOC(=O)C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
null
[Cu]I
C1CCOC1
Miscellaneous
OtherReaction
6586cb8fb9074fe79a2f08ccdc9c7ab8f943f0a45ff8db5202191123ff3bfd5e
81b73c69b19b4e45eeae7092f9c28fa5c915fb74eee9edf622d890bb40e4be14
C1CCNCC1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:5](=[CH;D2;+0:6]-[C:7](-[C:8])-[C:9])-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D3;+0:5](-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13])-[CH;D3;+0:6](-[C;D1;H3:14])-[C:7](-[C:8])-[C:9]
54.1
[{"value": 54.0, "product": "C(C)OC(C(C(=O)OCC)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 54.1, "product": "C(C)OC(C(C(=O)OCC)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
MeLi (5.34 mL, 8.54 mmol, 1.6 M in diethyl ether) was added dropwise to a slurry of CuI (0.74 g, 3.88 mmol) in THF (5 mL) at −78° C. under argon and the mixture was stirred for 30 min. A solution of 2-(1-tert-butoxycarbonyl-piperidin4-ylmethylene)-malonic acid diethyl ester (0.69 g, 1.94 mmol) in THF (5 mL) was added d...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ester.Ester
null
null
C1CC[NH]CC1
Other
[Cu]I.C1CCOC1
null
0.5
CCOC(=O)C(=CC1CCN(C(=O)OC(C)(C)C)CC1)C(=O)OCC>[Cu]I.C1CCOC1>CCOC(=O)C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c37643589f614cb7846bdd883ea6da7d
CCOC(=O)C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1>>CCOC(=O)C(C(=O)O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
[OH-].[K+].C(C)OC(C(C(=O)OCC)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O.CCOC(=O)C>>C(C)OC(C(C(=O)O)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O
CC[O:9][C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH:10]([CH3:11])[CH:12]1[CH2:13][CH2:14][N:15]([C:16](=[O:17])[O:18][C:19]([CH3:20])([CH3:21])[CH3:22])[CH2:23][CH2:24]1)=[O:8]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([C:7](=[O:8])[OH:9])[CH:10]([CH3:11])[CH:12]1[CH2:13][CH2:14][N:15]([C:16](=[O:17])[O:18][C:19]([C...
CCOC(=O)C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
CCOC(=O)C(C(=O)O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
null
null
C(Cl)Cl.CCO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
C1CCNCC1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
119.9
[{"value": 119.9, "product": "C(C)OC(C(C(=O)O)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of KOH (84 mg, 1.16 mmol) in EtOH (2 mL) was added dropwise to a solution of 2-[1-(1-tert-butoxycarbonyl-piperidin-4-yl)-ethyl]-malonic acid diethyl ester (0.39 g, 1.01 mmol) in methylene chloride (4 mL) and EtOH (10 mL) at 0° C. The resulting mixture was stirred at room temperature over night. EtOAc was add...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CC[NH]CC1
Other
C(Cl)Cl.CCO
null
null
CCOC(=O)C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1>C(Cl)Cl.CCO>CCOC(=O)C(C(=O)O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-38d871a641174a1f87aebfb6a9fb8167
CCOC(=O)C(C(=O)O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1>>C=C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
CCOC(=O)C.C=O.C(C)OC(C(C(=O)O)C(C)C1CCN(CC1)C(=O)OC(C)(C)C)=O.C(C)NCC>>C(C)(C)(C)OC(=O)N1CCC(CC1)C(C(=C)C(=O)OCC)C
O=[C:1](O)[CH:2]([C:3](=[O:4])[O:5][CH2:6][CH3:7])[CH:8]([CH3:9])[CH:10]1[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])[CH2:21][CH2:22]1>>[CH2:1]=[C:2]([C:3](=[O:4])[O:5][CH2:6][CH3:7])[CH:8]([CH3:9])[CH:10]1[CH2:11][CH2:12][N:13]([C:14](=[O:15])[O:16][C:17]([CH3:18])([CH3:19])[CH3:20])...
CCOC(=O)C(C(=O)O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
C=C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
485594ce7bba157615ffbb01ccede84a4e638576571b5d04649a06f3d4b7bce0
55e5b5078322f9f4fb0a7e9b5fc8a8cb9084e9135b447b8c441ad0800765792e
C1CCNCC1
O-[C;H0;D3;+0:1](=O)-[CH;D3;+0:2](-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6])-[C:7](-[C:8])-[C;D1;H3:9]>>[C:8]-[C:7](-[C;D1;H3:9])-[C;H0;D3;+0:2](=[CH2;D1;+0:1])-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6]
49
[{"value": 49.0, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)C(C(=C)C(=O)OCC)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 47.7, "product": "C(C)(C)(C)OC(=O)N1CCC(CC1)C(C(=C)C(=O)OCC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Formaldehyde (132 mg, 1.65 mmol, 37% in water) was added to a solution of of crude 2-[1-(1-tert-butoxycarbonyl-piperidin4-yl)-ethyl]-malonic acid monoethyl ester (416 mg) in methylene chloride (2 mL) at 0° C. Diethylamine (153 μL, 1.47 mmol) was added dropwise and the mixture was stirred at room temperature over night....
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester.Vinyl
null
null
C1CC[NH]CC1
Other
C(Cl)Cl
null
null
CCOC(=O)C(C(=O)O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1>C(Cl)Cl>C=C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b53a6ec53d094e5881ace0eea6d99552
C=C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1.CC(O)=S>>CCOC(=O)C(CSC(C)=O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
C(C)(C)(C)OC(=O)N1CCC(CC1)C(C(=C)C(=O)OCC)C.C(C)(=S)O.C(C)(=S)O.CCOC(=O)C>>C(C)(C)(C)OC(=O)N1CCC(CC1)C(C(CSC(C)=O)C(=O)OCC)C
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[CH2:7])[CH:12]([CH3:13])[CH:14]1[CH2:15][CH2:16][N:17]([C:18](=[O:19])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])[CH2:25][CH2:26]1.[S:8]=[C:9]([CH3:10])[OH:11]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH:12]([CH3:13])[CH:14]1[CH2:15][CH2:16][N:17]...
C=C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1.CC(O)=S
CCOC(=O)C(CSC(C)=O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
null
null
null
Protection
OtherReaction
56aa090d67fbecbea8a1963579cc34949775a09653b2b2f2795c609c60e70c77
5a9b0d631147b21b844b3c73866d1d81ab543538a176ebae28118ae7e39e572f
C1CCNCC1
[C;D1;H3:1]-[C;H0;D3;+0:2](-[OH;D1;+0:3])=[S;H0;D1;+0:4].[C:5]-[C:6](-[C;D1;H3:7])-[C;H0;D3;+0:8](=[CH2;D1;+0:9])-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]>>[C:5]-[C:6](-[C;D1;H3:7])-[CH;D3;+0:8](-[CH2;D2;+0:9]-[S;H0;D2;+0:4]-[C;H0;D3;+0:2](-[C;D1;H3:1])=[O;H0;D1;+0:3])-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13]
null
[]
45
CELSIUS
null
null
TEA (86 μL, 0.617 mmol) was added to a solution of 4-(2ethoxycarbonyl-1-methyl-allyl)-piperidine-1-carboxylic acid tert-butyl ester (0.18 g, 0.59 mmol) in thioacetic acid (2 mL) at 0° C. After stirring for 6 h more thioacetic acid (2 mL) was added and the mixture was stirred at 45° C. over night. EtOAc was added and th...
10.6084/m9.figshare.5104873.v1
null
Ester.Thiocarbonyl.Vinyl
Ester.Carbo-thioester
null
null
C1CC[NH]CC1
null
null
45
null
C=C(C(=O)OCC)C(C)C1CCN(C(=O)OC(C)(C)C)CC1.CC(O)=S>>CCOC(=O)C(CSC(C)=O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-9261c70df4e7495e965dc2f338370af3
CCOC(=O)C(CSC(C)=O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1>>CCOC(=O)C(CSC(C)=O)C(C)C1CCNCC1
C(=O)(C(F)(F)F)O.C(C)(C)(C)OC(=O)N1CCC(CC1)C(C(CSC(C)=O)C(=O)OCC)C>>C(C)OC(C(C(C)C1CCNCC1)CSC(C)=O)=O
CC(C)(C)OC(=O)[N:17]1[CH2:16][CH2:15][CH:14]([CH:12]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH3:13])[CH2:19][CH2:18]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7][S:8][C:9]([CH3:10])=[O:11])[CH:12]([CH3:13])[CH:14]1[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]1
CCOC(=O)C(CSC(C)=O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1
CCOC(=O)C(CSC(C)=O)C(C)C1CCNCC1
null
null
C(Cl)Cl
Reduction
Boc amine deprotection
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
C1CCNCC1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5]>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5]
80
[{"value": 54.0, "product": "C(C)OC(C(C(C)C1CCNCC1)CSC(C)=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 80.0, "product": "C(C)OC(C(C(C)C1CCNCC1)CSC(C)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
90
MINUTE
TFA (2 mL) was added to a solution of 4-(3-acetylsulfanyl-2-ethoxycarbonyl-1-methyl-propyl)-piperidine-1-carboxylic acid tert-butyl ester (0.17 g, 0.439 mmol) in methylene chloride (10 mL). The reaction was stirred for 90 min and concentrated under reduced pressure. The crude product was purified using HPLC (10→50% ace...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
C1CCNCC1
HO-
C(Cl)Cl
null
1.5
CCOC(=O)C(CSC(C)=O)C(C)C1CCN(C(=O)OC(C)(C)C)CC1>C(Cl)Cl>CCOC(=O)C(CSC(C)=O)C(C)C1CCNCC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4c6df6aa7f004641b5850608bb4b3299
CCOC(=O)C(CSC(C)=O)C(C)C1CCNCC1>>CC(C1CCNCC1)C(CS)C(=O)O
Cl.OC(=O)C(F)(F)F.C(C)OC(C(C(C)C1CCNCC1)CSC(C)=O)=O>>SCC(C(=O)O)C(C)C1CCNCC1
CC[O:14][C:12]([CH:9]([CH:2]([CH3:1])[CH:3]1[CH2:4][CH2:5][NH:6][CH2:7][CH2:8]1)[CH2:10][S:11]C(C)=O)=[O:13]>>[CH3:1][CH:2]([CH:3]1[CH2:4][CH2:5][NH:6][CH2:7][CH2:8]1)[CH:9]([CH2:10][SH:11])[C:12](=[O:13])[OH:14]
CCOC(=O)C(CSC(C)=O)C(C)C1CCNCC1
CC(C1CCNCC1)C(CS)C(=O)O
null
null
null
Reduction
OtherReaction
1bcd8cbb2f136b4bcba1690e9ba45c4e43c89ba76f0e22de82a7d3fe318c82a9
5654c46fe4cb226f88ec3c899c7f9be1825c357673ea686958f9ef4883ee1db3
C1CCNCC1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5]-[S;H0;D2;+0:6]-C(-C)=O>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[C:4]-[C:5]-[SH;D1;+0:6]
134.6
[{"value": 134.6, "product": "SCC(C(=O)O)C(C)C1CCNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Conc. hydrochloric acid (4 mL) was added to 2-acetylsulfanylmethyl-3-piperidin4-yl-butyric acid ethyl ester TFA salt (0.101 g, 0.252 mmol) under argon. The reaction was heated to reflux for 5 h and then concentrated under reduced pressure to give a diastereomeric mixture of the title compound (73.7 mg) as the hydrochlo...
10.6084/m9.figshare.5104873.v1
null
Ester.Carbo-thioester
Carboxylic acid.Aliphatic thiol
null
null
C1CCNCC1
HO-
null
null
null
CCOC(=O)C(CSC(C)=O)C(C)C1CCNCC1>>CC(C1CCNCC1)C(CS)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ef027323b7f14718817f3146fc9387e1
CC(C)(C)OC(=O)Nc1ccc(CO)cn1>>CC(C)(C)OC(=O)Nc1ccc(C=O)cn1
C(C)(C)(C)OC(NC1=NC=C(C=C1)CO)=O>>C(C)(C)(C)OC(NC1=NC=C(C=C1)C=O)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][cH:11][c:12]([CH2:13][OH:14])[cH:15][n:16]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][c:9]1[cH:10][cH:11][c:12]([CH:13]=[O:14])[cH:15][n:16]1
CC(C)(C)OC(=O)Nc1ccc(CO)cn1
CC(C)(C)OC(=O)Nc1ccc(C=O)cn1
null
null
CS(=O)C
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccncc1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
78
[{"value": 78.0, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)C=O)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 77.9, "product": "C(C)(C)(C)OC(NC1=NC=C(C=C1)C=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
45
MINUTE
5 (5-hydroxymethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (7.00 g, 31.2 mmol) was dissolved in dry DMSO (50 mL) and the reaction flask immersed in a waterbath at 15° C. TEA (13.1 ml, 94.0 mmol) was added, followed by sulfur trioxide pyridine complex (15.0 g, 94.0 mmol) in portions. The reaction mixture was stirre...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccncc1
null
CS(=O)C
null
0.75
CC(C)(C)OC(=O)Nc1ccc(CO)cn1>CS(=O)C>CC(C)(C)OC(=O)Nc1ccc(C=O)cn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-855ca57819ec4d568df1a98193a2fafc
CC(C)(C)OC(=O)Nc1ccc(C=O)cn1.CCOC(=O)CC(=O)OCC>>CCOC(=O)C(=Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
C(CC(=O)OCC)(=O)OCC.C(C)(C)(C)OC(NC1=NC=C(C=C1)C=O)=O.N1CCCCC1.C(C)(=O)O>>C(C)OC(C(C(=O)OCC)=CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
O=[CH:7][c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:19])[n:20][cH:21]1.[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:22](=[O:23])[O:24][CH2:25][CH3:26]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6](=[CH:7][c:8]1[cH:9][cH:10][c:11]([NH:12][C:13](=[O:14])[O:15][C:16]([CH3:17])([CH3:18])[CH3:...
CC(C)(C)OC(=O)Nc1ccc(C=O)cn1.CCOC(=O)CC(=O)OCC
CCOC(=O)C(=Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
null
null
CCCCCCC.C(Cl)Cl.CN(C)C=O
C-C Coupling
Aldol condensation
4308c3bc8a698ffc0b4a25652616c227140ef668f7c572096e661e9937e780ad
fae8d7810715ce1cb0ea563a010deed21a5c5db9b9f45a5f7ae1c022defa3e22
c1ccncc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[C;H0;D3;+0:11](=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
40.3
[{"value": 40.0, "product": "C(C)OC(C(C(=O)OCC)=CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 40.3, "product": "C(C)OC(C(C(=O)OCC)=CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
72
HOUR
To a solution of diethyl malonate (710 μL, 4.7 mmol) and (5-formyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.04 g, 4.7 mmol) in methylene chloride/DMF (1:1, 5 mL) was added piperidine (46 μL, 0.47 mmol) and acetic acid (27 μL, 0.47 mmol). The reaction mixture was stirred for 72 h at room temperature and then for ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester.Ester
Ester.Ester
null
null
c1ccncc1
HO-
CCCCCCC.C(Cl)Cl.CN(C)C=O
null
72
CC(C)(C)OC(=O)Nc1ccc(C=O)cn1.CCOC(=O)CC(=O)OCC>CCCCCCC.C(Cl)Cl.CN(C)C=O>CCOC(=O)C(=Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b2e368cb3ea14d72b8d97f1aee77e1cd
CCOC(=O)C(=Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC>>CCOC(=O)C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
[Li]C.C(C)OC(C(C(=O)OCC)=CC=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.[NH4+].[OH-]>>C(C)OC(C(C(=O)OCC)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([C:7](=[O:8])[O:9][CH2:10][CH3:11])=[CH:12][c:14]1[cH:15][cH:16][c:17]([NH:18][C:19](=[O:20])[O:21][C:22]([CH3:23])([CH3:24])[CH3:25])[n:26][cH:27]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([C:7](=[O:8])[O:9][CH2:10][CH3:11])[CH:12]([CH3:13])[c:14]1[cH:15][cH:16][c:17]([NH:18][C:19]...
CCOC(=O)C(=Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC
CCOC(=O)C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
null
[Cu]I
C1CCOC1
Miscellaneous
OtherReaction
6586cb8fb9074fe79a2f08ccdc9c7ab8f943f0a45ff8db5202191123ff3bfd5e
81b73c69b19b4e45eeae7092f9c28fa5c915fb74eee9edf622d890bb40e4be14
c1ccncc1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:5](=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9]:[#7;a:10]:[c:11])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D3;+0:5](-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15])-[CH;D3;+0:6](-[C;D1;H3:16])-[c:7](:[c:8]):[c:9]:[#7;a:10]:[c:11]
82.6
[{"value": 82.4, "product": "C(C)OC(C(C(=O)OCC)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 82.6, "product": "C(C)OC(C(C(=O)OCC)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
MeLi (6.5 mL, 10.4 mmol, 1.6 M in diethyl ether) was added dropwise to a slurry of CuI (0.9 g, 4.73 mmol) in THF (28 mL) at −78° C. under argon. The reaction mixture was stirred for 30 min. A solution of 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethylene)-malonic acid diethyl ester (0.84 g, 2.3 mmol) in THF (7 mL) was...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Ester.Ester
null
null
c1ccncc1
Other
[Cu]I.C1CCOC1
null
0.5
CCOC(=O)C(=Cc1ccc(NC(=O)OC(C)(C)C)nc1)C(=O)OCC>[Cu]I.C1CCOC1>CCOC(=O)C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cd61fcaf6d09420faf778f4a0e3fa1f3
CCOC(=O)C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1>>CCOC(=O)C(C(=O)O)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
[OH-].[K+].C(C)OC(C(C(=O)OCC)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.[OH-].[K+]>>C(C)OC(C(C(=O)O)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
CC[O:9][C:7]([CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH:10]([CH3:11])[c:12]1[cH:13][cH:14][c:15]([NH:16][C:17](=[O:18])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[n:24][cH:25]1)=[O:8]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([C:7](=[O:8])[OH:9])[CH:10]([CH3:11])[c:12]1[cH:13][cH:14][c:15]([NH:16][C:17](=[O:18])[O:19][C:2...
CCOC(=O)C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
CCOC(=O)C(C(=O)O)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
null
null
C(Cl)Cl.CCO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccncc1
C-C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[C:5](-[#8:6])=[O;D1;H0:7]>>[#8:6]-[C:5](=[O;D1;H0:7])-[C:4]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
65.2
[{"value": 65.0, "product": "C(C)OC(C(C(=O)O)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.2, "product": "C(C)OC(C(C(=O)O)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of KOH (113.6 mg, 2.04 mmol) in EtOH (2 mL) was added dropwise to a solution of 2-[1-(6-tert-butoxycarbonylamino-pyridin-3-yl)-ethyl]-malonic acid diethyl ester (0.7 g, 1.84 mmol) in methylene chloride (4 mL) and EtOH (10 mL) at 0° C. under argon and the reaction mixture was stirred over night. 1M KOH (100 m...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccncc1
Other
C(Cl)Cl.CCO
null
null
CCOC(=O)C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1>C(Cl)Cl.CCO>CCOC(=O)C(C(=O)O)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e8dccdb06f9e44fabf50426169d54b15
CCOC(=O)C(C(=O)O)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1>>C=C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
CCOC(=O)C.C(C)NCC.C(C)OC(C(C(=O)O)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O.C=O>>C(C)OC(C(=C)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O
O=[C:1](O)[CH:2]([C:3](=[O:4])[O:5][CH2:6][CH3:7])[CH:8]([CH3:9])[c:10]1[cH:11][cH:12][c:13]([NH:14][C:15](=[O:16])[O:17][C:18]([CH3:19])([CH3:20])[CH3:21])[n:22][cH:23]1>>[CH2:1]=[C:2]([C:3](=[O:4])[O:5][CH2:6][CH3:7])[CH:8]([CH3:9])[c:10]1[cH:11][cH:12][c:13]([NH:14][C:15](=[O:16])[O:17][C:18]([CH3:19])([CH3:20])[CH3...
CCOC(=O)C(C(=O)O)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
C=C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
485594ce7bba157615ffbb01ccede84a4e638576571b5d04649a06f3d4b7bce0
55e5b5078322f9f4fb0a7e9b5fc8a8cb9084e9135b447b8c441ad0800765792e
c1ccncc1
O-[C;H0;D3;+0:1](=O)-[CH;D3;+0:2](-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6])-[C:7](-[C;D1;H3:8])-[c:9]:[c:10]:[#7;a:11]>>[#7;a:11]:[c:10]:[c:9]-[C:7](-[C;D1;H3:8])-[C;H0;D3;+0:2](=[CH2;D1;+0:1])-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6]
41.1
[{"value": 41.0, "product": "C(C)OC(C(=C)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 41.1, "product": "C(C)OC(C(=C)C(C)C=1C=NC(=CC1)NC(=O)OC(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Diethylamine (0.153 mL, 1.473 mmol) was added to a solution of 2-[1-(6-tert-butoxycarbonylamino-pyridin-3-yl)-ethyl]-malonic acid monoethyl ester (423 mg, 1.2 mmol) and formaldehyde (132 mg, 1.626 mmol, 36% in water) in methylene chloride (2 mL) at 0° C. under argon. The mixture was stirred at room temperature over nig...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester
Ester.Vinyl
null
null
c1ccncc1
Other
C(Cl)Cl
null
null
CCOC(=O)C(C(=O)O)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1>C(Cl)Cl>C=C(C(=O)OCC)C(C)c1ccc(NC(=O)OC(C)(C)C)nc1