dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
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
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
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-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6c62f99d0fed4032b2e1262e33a10198
CC(C)(C)c1ccc(S(N)(=O)=O)cc1.Clc1cc(Cl)ncn1>>CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(Cl)ncn2)cc1
ClC1=NC=NC(=C1)Cl.C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)N.[H-].[Na+]>>C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)NC1=NC=NC(=C1)Cl
[CH3:1][C:2]([CH3:3])([CH3:4])[c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[NH2:12])[cH:20][cH:21]1.Cl[c:13]1[cH:14][c:15]([Cl:16])[n:17][cH:18][n:19]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[NH:12][c:13]2[cH:14][c:15]([Cl:16])[n:17][cH:18][n:19]2)[cH:20][cH:21]1
CC(C)(C)c1ccc(S(N)(=O)=O)cc1.Clc1cc(Cl)ncn1
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(Cl)ncn2)cc1
null
null
CN(C=O)C.Cl.O
Heteroatom Alkylation and Arylation
OtherReaction
345edf40ad678aea0250ec5b3d6cc512d8eac020b2f4324f423c18b59726753e
e7974806b40218fa965bb62bf9c430cac38870897b20726116f8b48ae128dc55
O=S(=O)(Nc1ccncn1)c1ccccc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[Cl;D1;H0:6]):[c:7]:1.[NH2;D1;+0:8]-[#16:9](=[O;D1;H0:10])(=[O;D1;H0:11])-[c:12]>>[Cl;D1;H0:6]-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:8]-[#16:9](=[O;D1;H0:10])(=[O;D1;H0:11])-[c:12]):[c:7]:1
69.4
[{"value": 69.4, "product": "C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)NC1=NC=NC(=C1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of 4,6-dichloropyrimidine (1.33 g) and 4-tert-butylbenzenesulfonamide (1.96 g) in dimethylformamide (20 ml) is added sodium hydride (60% dispersion-type, 714 mg). The mixture is stirred at room temperature for two hours, and the reaction solution is diluted with 10% hydrochloric acid and water. The mixtur...
10.6084/m9.figshare.5104873.v1
null
Sulfonamide.Aromatic halide
Sulfonamide
c1cncnc1
c1cncnc1
c1ccccc1.c1cncnc1
HCl
CN(C=O)C.Cl.O
null
2
CC(C)(C)c1ccc(S(N)(=O)=O)cc1.Clc1cc(Cl)ncn1>CN(C=O)C.Cl.O>CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(Cl)ncn2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a389d63ceeae4459863ae17f76d2bba8
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(Cl)ncn2)cc1.OCCO>>CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(OCCO)ncn2)cc1
C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)NC1=NC=NC(=C1)Cl.[H-].[Na+].C(CO)O.Cl>>C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)NC1=NC=NC(=C1)OCCO
Cl[c:15]1[cH:14][c:13]([NH:12][S:9]([c:8]2[cH:7][cH:6][c:5]([C:2]([CH3:1])([CH3:3])[CH3:4])[cH:24][cH:23]2)(=[O:10])=[O:11])[n:22][cH:21][n:20]1.[OH:16][CH2:17][CH2:18][OH:19]>>[CH3:1][C:2]([CH3:3])([CH3:4])[c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[NH:12][c:13]2[cH:14][c:15]([O:16][CH2:17][CH2:18][OH:19])[n:20][c...
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(Cl)ncn2)cc1.OCCO
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(OCCO)ncn2)cc1
null
null
null
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
a445000eb5ed501274d93689ad5b9d45095af02deca02b6b541c8a834890a276
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
O=S(=O)(Nc1ccncn1)c1ccccc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[#7:6]):[c:7]:1.[C:8]-[C:9]-[OH;D1;+0:10]>>[#7:6]-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[O;H0;D2;+0:10]-[C:9]-[C:8]):[c:7]:1
null
[]
60
CELSIUS
20
HOUR
To ethylene glycol (20 ml) is added sodium hydride (60% dispersion-type, 1.03 g), and thereto is added 4-tert-butyl-N-(6-chloropyrimidin-4-yl)benzenesulfonamide (1.66 g). The mixture is stirred at 60° C. for 20 hours. After cooling, the mixture is acidified with 10% hydrochloric acid, and extracted with ethyl acetate. ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cncnc1
c1cncnc1
c1ccccc1.c1cncnc1
HCl
null
60
20
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(Cl)ncn2)cc1.OCCO>>CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(OCCO)ncn2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-da9e15d8493a44cfbbae58022cf084ac
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(OCCO)ncn2)cc1.O=C1CCC(=O)N1Br>>CC(C)(C)c1ccc(S(=O)(=O)Nc2ncnc(OCCO)c2Br)cc1
S(=O)(O)[O-].[Na+].C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)NC1=NC=NC(=C1)OCCO.BrN1C(CCC1=O)=O>>BrC=1C(=NC=NC1OCCO)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C
[CH3:1][C:2]([CH3:3])([CH3:4])[c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[NH:12][c:13]2[n:14][cH:15][n:16][c:17]([O:18][CH2:19][CH2:20][OH:21])[cH:22]2)[cH:24][cH:25]1.O=C1CCC(=O)N1[Br:23]>>[CH3:1][C:2]([CH3:3])([CH3:4])[c:5]1[cH:6][cH:7][c:8]([S:9](=[O:10])(=[O:11])[NH:12][c:13]2[n:14][cH:15][n:16][c:17]([O:18][CH...
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(OCCO)ncn2)cc1.O=C1CCC(=O)N1Br
CC(C)(C)c1ccc(S(=O)(=O)Nc2ncnc(OCCO)c2Br)cc1
null
null
CN(C=O)C
Functional Group Interconversion
Bromination
ce862b99084d022122186a4bb29e2cc909823387b5fab03ae9d40a04a60bbc3f
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
O=S(=O)(Nc1ccncn1)c1ccccc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[#7:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7](-[#8:8]):[cH;D2;+0:9]:1>>[#7:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7](-[#8:8]):[c;H0;D3;+0:9]:1-[Br;H0;D1;+0:1]
65.7
[{"value": 65.7, "product": "BrC=1C(=NC=NC1OCCO)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 4-tert-butyl-N-[6-(2-hydroxyethoxy)pyrimidin-4-yl)benzenesulfonamide (210 mg) in dimethylformamide (4 ml) is added N-bromosuccinimide (116 mg), and the mixture is stirred at room temperature for one hour. The mixture is treated with aqueous sodium hydrogen sulfite solution, and extracted with ethyl ace...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1cncnc1.C1CCNC1
c1cncnc1
c1ccccc1.c1cncnc1
HO-
CN(C=O)C
null
1
CC(C)(C)c1ccc(S(=O)(=O)Nc2cc(OCCO)ncn2)cc1.O=C1CCC(=O)N1Br>CN(C=O)C>CC(C)(C)c1ccc(S(=O)(=O)Nc2ncnc(OCCO)c2Br)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b4685538e6b8446fb9eabb0b5495e015
CC(C)(C)c1ccc(S(=O)(=O)Nc2ncnc(OCCO)c2Br)cc1.CSc1cnc(Cl)nc1>>CSc1cnc(OCCOc2ncnc(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)c2Br)nc1
BrC=1C(=NC=NC1OCCO)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C.[H-].[Na+].Cl.[Cl-].[NH4+].ClC1=NC=C(C=N1)SC>>BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C
[OH:7][CH2:8][CH2:9][O:10][c:11]1[n:12][cH:13][n:14][c:15]([NH:16][S:17](=[O:18])(=[O:19])[c:20]2[cH:21][cH:22][c:23]([C:24]([CH3:25])([CH3:26])[CH3:27])[cH:28][cH:29]2)[c:30]1[Br:31].Cl[c:6]1[n:5][cH:4][c:3]([S:2][CH3:1])[cH:33][n:32]1>>[CH3:1][S:2][c:3]1[cH:4][n:5][c:6]([O:7][CH2:8][CH2:9][O:10][c:11]2[n:12][cH:13][n...
CC(C)(C)c1ccc(S(=O)(=O)Nc2ncnc(OCCO)c2Br)cc1.CSc1cnc(Cl)nc1
CSc1cnc(OCCOc2ncnc(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)c2Br)nc1
null
null
CC(=O)N(C)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
a445000eb5ed501274d93689ad5b9d45095af02deca02b6b541c8a834890a276
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
O=S(=O)(Nc1cc(OCCOc2ncccn2)ncn1)c1ccccc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[C:6]-[C:7]-[OH;D1;+0:8]>>[C:6]-[C:7]-[O;H0;D2;+0:8]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5]
83.6
[{"value": 83.6, "product": "BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of N-[5-bromo-6-(2-hydroxyethoxy)pyrimidin-4-yl]-4-tert-butylbenzenesulfonamide (3.10 g) in dimethylacetamide (30 ml) is added sodium hydride (60% dispersion-type, 720 mg), and the mixture is stirred at room temperature for 30 minutes. To the mixture is added 2-chloro-5-methylthiopyrimidine (1.51 g), and ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cncnc1
c1cncnc1
c1cncnc1.c1cncnc1.c1ccccc1
HCl
CC(=O)N(C)C
null
0.5
CC(C)(C)c1ccc(S(=O)(=O)Nc2ncnc(OCCO)c2Br)cc1.CSc1cnc(Cl)nc1>CC(=O)N(C)C>CSc1cnc(OCCOc2ncnc(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)c2Br)nc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f570953042144533ac7122491f64e455
Clc1cc(Cl)ncn1.OCCO>>OCCOc1cc(Cl)ncn1
ClC1=NC=NC(=C1)Cl.C(CO)O.[H-].[Na+]>>ClC1=CC(=NC=N1)OCCO
Cl[c:5]1[cH:6][c:7]([Cl:8])[n:9][cH:10][n:11]1.[OH:1][CH2:2][CH2:3][OH:4]>>[OH:1][CH2:2][CH2:3][O:4][c:5]1[cH:6][c:7]([Cl:8])[n:9][cH:10][n:11]1
Clc1cc(Cl)ncn1.OCCO
OCCOc1cc(Cl)ncn1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
a445000eb5ed501274d93689ad5b9d45095af02deca02b6b541c8a834890a276
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1cncnc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[Cl;D1;H0:6]):[c:7]:1.[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]:[#7;a:4]:[c:5](-[Cl;D1;H0:6]):[c:7]:1
null
[]
null
null
2
HOUR
To a mixture of 4,6-dichloropyrimidine (5.0 g), ethylene glycol (100 ml) and tetrahydrofuran (100 ml)is added sodium hydride (60% dispersion-type, 1.34 g) under ice-cooling. The mixture is stirred at the same temperature for two hours, and evaporated to remove the solvent. The residue is extracted with ethyl acetate, a...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cncnc1
c1cncnc1
c1cncnc1
HCl
O1CCCC1
null
2
Clc1cc(Cl)ncn1.OCCO>O1CCCC1>OCCOc1cc(Cl)ncn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-fca1a49f76c14ce8bae2a93158f456ab
OCCOc1cc(Cl)ncn1.[N-]=[N+]=[N-]>>[N-]=[N+]=Nc1cc(OCCO)ncn1
O.ClC1=CC(=NC=N1)OCCO.[N-]=[N+]=[N-].[Na+]>>N(=[N+]=[N-])C1=CC(=NC=N1)OCCO
Cl[c:4]1[cH:5][c:6]([O:7][CH2:8][CH2:9][OH:10])[n:11][cH:12][n:13]1.[N-:1]=[N+:2]=[N-:3]>>[N-:1]=[N+:2]=[N:3][c:4]1[cH:5][c:6]([O:7][CH2:8][CH2:9][OH:10])[n:11][cH:12][n:13]1
OCCOc1cc(Cl)ncn1.[N-]=[N+]=[N-]
[N-]=[N+]=Nc1cc(OCCO)ncn1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
48465a5e07f474e518aa4021a9b68659838d8b370bfeed26501047d7c300e8e7
df579c5e1cf1cc42720dad6dd16c8deec88e9170508fbd47357453cfc40bcb7a
c1cncnc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[#8:6]):[c:7]:1.[N-;H0;D1:8]=[#7;+:9]=[N;-;D1;H0:10]>>[#8:6]-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[N;H0;D2;+0:8]=[#7;+:9]=[N;-;D1;H0:10]):[c:7]:1
28.9
[{"value": 28.9, "product": "N(=[N+]=[N-])C1=CC(=NC=N1)OCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
20
HOUR
To a solution of 2-(6-chloropyrimidin-4-yloxy)ethanol (5.61 g) in dimethylformamide (60 ml) is added sodium azide (4.18 g), and the mixture is stirred at 70° C. for 20 hours. After cooling, the reaction solution is treated with water, and extracted with ethyl acetate. The ethyl acetate layer is dried, and evaporated to...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Azide
c1cncnc1
c1cncnc1
c1cncnc1
Other
CN(C=O)C
70
20
OCCOc1cc(Cl)ncn1.[N-]=[N+]=[N-]>CN(C=O)C>[N-]=[N+]=Nc1cc(OCCO)ncn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-fa1f51d360144913905861053111ec80
[N-]=[N+]=Nc1cc(OCCO)ncn1>>Nc1cc(OCCO)ncn1
N(=[N+]=[N-])C1=CC(=NC=N1)OCCO>>NC1=CC(=NC=N1)OCCO
[N-]=[N+]=[N:1][c:2]1[cH:3][c:4]([O:5][CH2:6][CH2:7][OH:8])[n:9][cH:10][n:11]1>>[NH2:1][c:2]1[cH:3][c:4]([O:5][CH2:6][CH2:7][OH:8])[n:9][cH:10][n:11]1
[N-]=[N+]=Nc1cc(OCCO)ncn1
Nc1cc(OCCO)ncn1
null
[C].[Pd]
C(C)O
Reduction
Azide to amine reduction (Staudinger)
4c9e4990dae2bb965dec06bd45e318560989ee3681b61e443f7aa363b7cfa222
cd009d687d606bf351eac9390a176d16be38f2c8216a599b398641009c215027
c1cncnc1
[N-]=[N+]=[N;H0;D2;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1>>[NH2;D1;+0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:[c:7]:1
79
[{"value": 79.0, "product": "NC1=CC(=NC=N1)OCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
A mixture of 2-(6-azidopyrimidin-4-yloxy)ethanol (1.64 g), 10% palladium-carbon (0.25 g) and ethanol (20 ml) is subjected to catalytic hydrogenation at room temperature for one hour under hydrogen atmosphere (1 atm). The catalyst is removed by filtration, and the filtrate is concentrated. The residue is recrystallized ...
10.6084/m9.figshare.5104873.v1
null
Azide
Primary amine
null
null
c1cncnc1
Other
[C].[Pd].C(C)O
null
1
[N-]=[N+]=Nc1cc(OCCO)ncn1>[C].[Pd].C(C)O>Nc1cc(OCCO)ncn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2f3278729434431a9be2a0b527dc71ea
BrBr.Nc1cc(OCCO)ncn1>>Nc1ncnc(OCCO)c1Br
NC1=CC(=NC=N1)OCCO.BrBr>>NC1=C(C(=NC=N1)OCCO)Br
Br[Br:12].[NH2:1][c:2]1[n:3][cH:4][n:5][c:6]([O:7][CH2:8][CH2:9][OH:10])[cH:11]1>>[NH2:1][c:2]1[n:3][cH:4][n:5][c:6]([O:7][CH2:8][CH2:9][OH:10])[c:11]1[Br:12]
BrBr.Nc1cc(OCCO)ncn1
Nc1ncnc(OCCO)c1Br
null
null
CO
Functional Group Interconversion
Bromination
b0bb6940bdaa4f483f95617a9ee5e6563c160ea710db3fde10ee056459a3fce1
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1cncnc1
Br-[Br;H0;D1;+0:1].[#8:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7](-[N;D1;H2:8]):[cH;D2;+0:9]:1>>[#8:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7](-[N;D1;H2:8]):[c;H0;D3;+0:9]:1-[Br;H0;D1;+0:1]
104.7
[{"value": 104.7, "product": "NC1=C(C(=NC=N1)OCCO)Br", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of 2-(6-aminopyrimidin-4-yloxy)ethanol (400 mg) in methanol (4 ml) is added dropwise a solution of bromine (437 mg) in methanol (2 ml). The mixture is evaporated to remove the solvent, and the residue is dissolved in ethyl acetate. The mixture is treated with saturated aqueous sodium hydrogen carbonate ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cncnc1
c1cncnc1
c1cncnc1
HBr
CO
null
null
BrBr.Nc1cc(OCCO)ncn1>CO>Nc1ncnc(OCCO)c1Br
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4bd91debc1224985b59b17dd05823067
CSc1cnc(Cl)nc1.Nc1ncnc(OCCO)c1Br>>CSc1cnc(OCCOc2ncnc(N)c2Br)nc1
ClC1=NC=C(C=N1)SC.NC1=C(C(=NC=N1)OCCO)Br.[H-].[Na+]>>BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)N
Cl[c:6]1[n:5][cH:4][c:3]([S:2][CH3:1])[cH:20][n:19]1.[OH:7][CH2:8][CH2:9][O:10][c:11]1[n:12][cH:13][n:14][c:15]([NH2:16])[c:17]1[Br:18]>>[CH3:1][S:2][c:3]1[cH:4][n:5][c:6]([O:7][CH2:8][CH2:9][O:10][c:11]2[n:12][cH:13][n:14][c:15]([NH2:16])[c:17]2[Br:18])[n:19][cH:20]1
CSc1cnc(Cl)nc1.Nc1ncnc(OCCO)c1Br
CSc1cnc(OCCOc2ncnc(N)c2Br)nc1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
a445000eb5ed501274d93689ad5b9d45095af02deca02b6b541c8a834890a276
a4cafa7bcd156e21cca6eaac1b32e28ec8540642a31181122e6957f3d7559631
c1cnc(OCCOc2ccncn2)nc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[C:6]-[C:7]-[OH;D1;+0:8]>>[C:6]-[C:7]-[O;H0;D2;+0:8]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5]
53.6
[{"value": 53.6, "product": "BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of 2-(6-amino-5-bromopyrimidin-4-yloxy)ethanol (611 mg) in dimethylformamide (20 ml) is added sodium hydride (60% dispersion-type, 125 mg), and the mixture is stirred for 20 minutes. To the mixture is added 2-chloro-5-methylthiopyrimidine (461 mg), and the mixture is stirred at room temperature for three ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary alcohol
Ether
c1cncnc1
c1cncnc1
c1cncnc1.c1cncnc1
HCl
CN(C=O)C
null
0.333333
CSc1cnc(Cl)nc1.Nc1ncnc(OCCO)c1Br>CN(C=O)C>CSc1cnc(OCCOc2ncnc(N)c2Br)nc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ad49e82362d34ffea232b146b2698729
CC(C)(C)c1ccc(S(=O)(=O)Cl)cc1.CSc1cnc(OCCOc2ncnc(N)c2Br)nc1>>CSc1cnc(OCCOc2ncnc(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)c2Br)nc1
[Cl-].[NH4+].C(C)(C)(C)C1=CC=C(C=C1)S(=O)(=O)Cl.BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)N.[H-].[Na+]>>BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C
Cl[S:17](=[O:18])(=[O:19])[c:20]1[cH:21][cH:22][c:23]([C:24]([CH3:25])([CH3:26])[CH3:27])[cH:28][cH:29]1.[CH3:1][S:2][c:3]1[cH:4][n:5][c:6]([O:7][CH2:8][CH2:9][O:10][c:11]2[n:12][cH:13][n:14][c:15]([NH2:16])[c:30]2[Br:31])[n:32][cH:33]1>>[CH3:1][S:2][c:3]1[cH:4][n:5][c:6]([O:7][CH2:8][CH2:9][O:10][c:11]2[n:12][cH:13][n...
CC(C)(C)c1ccc(S(=O)(=O)Cl)cc1.CSc1cnc(OCCOc2ncnc(N)c2Br)nc1
CSc1cnc(OCCOc2ncnc(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)c2Br)nc1
null
null
N1=CC=CC=C1.O.O1CCCC1
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=S(=O)(Nc1cc(OCCOc2ncccn2)ncn1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[NH2;D1;+0:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]:[c:13]:1>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]:[c:13]:1)-[c:4](:[c:5]):[c:6]
85.5
[{"value": 85.5, "product": "BrC=1C(=NC=NC1OCCOC1=NC=C(C=N1)SC)NS(=O)(=O)C1=CC=C(C=C1)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of 5-bromo-6-[2-(5-methylthiopyrimidin-2-yloxy)ethoxy]pyrimidine-4-amine (102 mg) in tetrahydrofuran (2 ml) is added sodium hydride (60% dispersion-type, 34 mg), and thereto is added 4-tert-butylbenzenesulfonyl chloride (198 mg). The mixture is stirred at room temperature for 20 minutes, and thereto are a...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1cncnc1.c1cncnc1.c1ccccc1
HCl
N1=CC=CC=C1.O.O1CCCC1
null
0.333333
CC(C)(C)c1ccc(S(=O)(=O)Cl)cc1.CSc1cnc(OCCOc2ncnc(N)c2Br)nc1>N1=CC=CC=C1.O.O1CCCC1>CSc1cnc(OCCOc2ncnc(NS(=O)(=O)c3ccc(C(C)(C)C)cc3)c2Br)nc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-fcdab10bc84144e59957a7d86566aed7
CCCC(=N)N.CCOC(=O)C(C(=O)OCC)c1ccc(C)cc1>>CCCc1nc(O)c(-c2ccc(C)cc2)c(O)n1
C(C)OC(C(C(=O)OCC)C1=CC=C(C=C1)C)=O.Cl.C(CCC)(=N)N.C[O-].[Na+]>>CC1=CC=C(C=C1)C=1C(=NC(=NC1O)CCC)O
[CH3:1][CH2:2][CH2:3][C:4](=[NH:5])[NH2:18].CCO[C:6](=[O:7])[CH:8]([c:9]1[cH:10][cH:11][c:12]([CH3:13])[cH:14][cH:15]1)[C:16](OCC)=[O:17]>>[CH3:1][CH2:2][CH2:3][c:4]1[n:5][c:6]([OH:7])[c:8](-[c:9]2[cH:10][cH:11][c:12]([CH3:13])[cH:14][cH:15]2)[c:16]([OH:17])[n:18]1
CCCC(=N)N.CCOC(=O)C(C(=O)OCC)c1ccc(C)cc1
CCCc1nc(O)c(-c2ccc(C)cc2)c(O)n1
null
null
CO
Aromatic Heterocycle Formation
OtherReaction
d507ea5e988c6bcfe927f1b3a86f934f8a1c706f38171153cdf4dbd7aeb28e83
6504f33921726f64e36c5f3f322459b73652319c83071522ec21b8b88a33a5a7
c1ccc(-c2cncnc2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[CH;D3;+0:3](-[C;H0;D3;+0:4](=[O;H0;D1;+0:5])-O-C-C)-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:9]:[c:10].[C:11]-[C:12]-[C;H0;D3;+0:13](-[NH2;D1;+0:14])=[NH;D1;+0:15]>>[C:11]-[C:12]-[c;H0;D3;+0:13]1:[n;H0;D2;+0:14]:[c;H0;D3;+0:1](-[OH;D1;+0:2]):[c;H0;D3;+0:3](-[c;H0;D3;+0:6](:[c:7]:[c:8]):[c:...
56.1
[{"value": 56.1, "product": "CC1=CC=C(C=C1)C=1C(=NC(=NC1O)CCC)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of diethyl(4-methylphenyl)malonate (9.45 g) and butyramidine hydrochloride (5.00 g) in methanol (25 ml) is added 28% sodium methoxide (19.67 g) under ice-cooling, and the mixture is stirred at room temperature overnight. After the reaction is complete, the reaction solution is concentrated to the half vol...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Primary amine
Aromatic alcohol.Aromatic alcohol
null
c1cncnc1
c1cncnc1.c1ccccc1
HO-
CO
null
8
CCCC(=N)N.CCOC(=O)C(C(=O)OCC)c1ccc(C)cc1>CO>CCCc1nc(O)c(-c2ccc(C)cc2)c(O)n1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1ce4869becc14147b48b50fb8a727e75
Cc1ccc(-c2c(Cl)ncnc2Cl)cc1.c1ccsc1>>Cc1ccc(-c2c(Cl)nc(-c3cccs3)nc2Cl)cc1
S1C=CC=C1.C(CCC)[Li].CCCCCC.ClC=1C(C(=C(C(C1Cl)=O)C#N)C#N)=O.C.CC1=CC=C(C=C1)C=1C(=NC=NC1Cl)Cl>>CC1=CC=C(C=C1)C=1C(=NC(=NC1Cl)C=1SC=CC1)Cl
[CH3:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[c:7]([Cl:8])[n:9][cH:10][n:16][c:17]2[Cl:18])[cH:19][cH:20]1.[cH:11]1[cH:12][cH:13][cH:14][s:15]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[c:7]([Cl:8])[n:9][c:10](-[c:11]3[cH:12][cH:13][cH:14][s:15]3)[n:16][c:17]2[Cl:18])[cH:19][cH:20]1
Cc1ccc(-c2c(Cl)ncnc2Cl)cc1.c1ccsc1
Cc1ccc(-c2c(Cl)nc(-c3cccs3)nc2Cl)cc1
null
null
C(C)(=O)O.O.O1CCCC1
C-C Coupling
OtherReaction
7477d571945f2e3c2b5e66e8121ec6c1e6cb8c3c83feee0f74fa4cf43ecd0b4c
410ec9b1cc243569e4ff568c248f0b402403802e002b4018f576af3f6960507b
c1ccc(-c2cnc(-c3cccs3)nc2)cc1
[#16;a:1]1:[c:2]:[c:3]:[c:4]:[cH;D2;+0:5]:1.[c:6]:[#7;a:7]:[cH;D2;+0:8]:[#7;a:9]:[c:10]>>[c:6]:[#7;a:7]:[c;H0;D3;+0:8](-[c;H0;D3;+0:5]1:[#16;a:1]:[c:2]:[c:3]:[c:4]:1):[#7;a:9]:[c:10]
49.1
[{"value": 49.1, "product": "CC1=CC=C(C=C1)C=1C(=NC(=NC1Cl)C=1SC=CC1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
1.5
HOUR
To a solution of thiophene (1.69 g) in anhydrous tetrahydrofuran (20 ml) is added dropwise a 1.6M n-butyl lithium/n-hexane solution (11.4 ml) at 0° C. under argon atmosphere over a period of 30 minutes. To the mixture is added dropwise and gradually a solution of 5-(4-methylphenyl)-4,6-dichloropyrimidine (4.0 g) in anh...
10.6084/m9.figshare.5104873.v1
null
null
null
c1cncnc1.c1ccsc1
c1cncnc1.c1ccsc1
c1ccccc1.c1cncnc1.c1ccsc1
null
C(C)(=O)O.O.O1CCCC1
0
1.5
Cc1ccc(-c2c(Cl)ncnc2Cl)cc1.c1ccsc1>C(C)(=O)O.O.O1CCCC1>Cc1ccc(-c2c(Cl)nc(-c3cccs3)nc2Cl)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-92159ddf5fca43a09bd60ede97b3d342
Cc1ccc(-c2c(Cl)ncnc2Cl)cc1.[Li][c]1ccccc1>>Cc1ccc(-c2c(Cl)nc(-c3ccccc3)nc2Cl)cc1
CC1=CC=C(C=C1)C=1C(=NC=NC1Cl)Cl.C1(=CC=CC=C1)[Li].C1CCCCC1>>CC1=CC=C(C=C1)C=1C(=NC(=NC1Cl)C1=CC=CC=C1)Cl
[CH3:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[c:7]([Cl:8])[n:9][cH:10][n:17][c:18]2[Cl:19])[cH:20][cH:21]1.[Li][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[c:7]([Cl:8])[n:9][c:10](-[c:11]3[cH:12][cH:13][cH:14][cH:15][cH:16]3)[n:17][c:18]2[Cl:19])[cH:20][cH:21]1
Cc1ccc(-c2c(Cl)ncnc2Cl)cc1.[Li][c]1ccccc1
Cc1ccc(-c2c(Cl)nc(-c3ccccc3)nc2Cl)cc1
null
null
CCOCC
C-C Coupling
OtherReaction
9a72b30d15d3a170453b5c35266e9d70841a0bbb9087716a1c585ee74f1223ea
cc013e751ce1c06538b7045e86b7a6f2058a4a034157294a153dbe8bc23160ba
c1ccc(-c2cnc(-c3ccccc3)nc2)cc1
[Li]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[c:6]:[#7;a:7]:[cH;D2;+0:8]:[#7;a:9]:[c:10]>>[c:3]:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:8](:[#7;a:7]:[c:6]):[#7;a:9]:[c:10]):[c:4]:[c:5]
null
[]
null
null
null
null
A solution of 5-(4-methylphenyl)-4,6-dichloropyrimidine in ether is cooled at -30° C., and thereto is added dropwise a 1.8M phenyl lithium/cyclohexane solution. The reaction mixture is treated in the same manner as in Reference Example 20-(1) to give 5-(4-methylphenyl)-4,6-dichloro-2-phenylpyrimidine as crystalline pow...
10.6084/m9.figshare.5104873.v1
null
Aryl lithium
null
c1cncnc1.c1ccccc1
c1cncnc1.c1ccccc1
c1ccccc1.c1cncnc1.c1ccccc1
Li
CCOCC
null
null
Cc1ccc(-c2c(Cl)ncnc2Cl)cc1.[Li][c]1ccccc1>CCOCC>Cc1ccc(-c2c(Cl)nc(-c3ccccc3)nc2Cl)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1f983a1da36340b0869e30cda784fc40
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccco1.Clc1ncc(Br)cn1>>Clc1ncc(-c2ccco2)cn1
ClC1=NC=C(C=N1)Br.O1C(=CC=C1)[Sn](CCCC)(CCCC)CCCC>>ClC1=NC=C(C=N1)C=1OC=CC1
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c:6]1[cH:7][cH:8][cH:9][o:10]1.Br[c:5]1[cH:4][n:3][c:2]([Cl:1])[n:12][cH:11]1>>[Cl:1][c:2]1[n:3][cH:4][c:5](-[c:6]2[cH:7][cH:8][cH:9][o:10]2)[cH:11][n:12]1
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccco1.Clc1ncc(Br)cn1
Clc1ncc(-c2ccco2)cn1
null
null
null
C-C Coupling
Stille reaction_aryl
521e946f48ccffcbe6b23a0e1f700a0148118f44680a29c08207616fca9cfae6
db27eeefac0475c6d74fa10b3167e95a61caaae74e8bbafd45892452c0c3d4d6
c1coc(-c2cncnc2)c1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1.C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[c;H0;D3;+0:7]1:[#8;a:8]:[c:9]:[c:10]:[c:11]:1>>[#7;a:3]1:[c:2]:[c;H0;D3;+0:1](-[c;H0;D3;+0:7]2:[#8;a:8]:[c:9]:[c:10]:[c:11]:2):[c:6]:[#7;a:5]:[c:4]:1
null
[]
null
null
null
null
2-Chloro-5-bromopyrimidine and 2-furyltributyltin are treated in the same manner as in Example 190 to give 2-chloro-5-(2-furyl)pyrimidine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tin
null
c1ccoc1.c1cncnc1
c1cncnc1.c1ccoc1
c1cncnc1.c1ccoc1
HBr.Sn
null
null
null
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccco1.Clc1ncc(Br)cn1>>Clc1ncc(-c2ccco2)cn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-1e36bdd34f9c40229a1193bb06a3ce85
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccsc1.Clc1ncc(Br)cn1>>Clc1ncc(-c2ccsc2)cn1
ClC1=NC=C(C=N1)Br.S1C=C(C=C1)[Sn](CCCC)(CCCC)CCCC>>ClC1=NC=C(C=N1)C1=CSC=C1
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c:6]1[cH:7][cH:8][s:9][cH:10]1.Br[c:5]1[cH:4][n:3][c:2]([Cl:1])[n:12][cH:11]1>>[Cl:1][c:2]1[n:3][cH:4][c:5](-[c:6]2[cH:7][cH:8][s:9][cH:10]2)[cH:11][n:12]1
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccsc1.Clc1ncc(Br)cn1
Clc1ncc(-c2ccsc2)cn1
null
null
null
C-C Coupling
Stille reaction_aryl
199420dc5768b1af27f86d7ad18eaf1b793cb98fd661ec8a8f552e8c67ad2d1d
db27eeefac0475c6d74fa10b3167e95a61caaae74e8bbafd45892452c0c3d4d6
c1ncc(-c2ccsc2)cn1
Br-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1.C-C-C-[CH2]-[Sn](-[CH2]-C-C-C)(-[CH2]-C-C-C)-[c;H0;D3;+0:7]1:[c:8]:[#16;a:9]:[c:10]:[c:11]:1>>[#16;a:9]1:[c:8]:[c;H0;D3;+0:7](-[c;H0;D3;+0:1]2:[c:2]:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:2):[c:11]:[c:10]:1
null
[]
null
null
null
null
2-Chloro-5-bromopyrimidine and 3-thienyltributyltin are treated in the same manner as in Example 190 to give 2-chloro-5-(3-thienyl)pyrimidine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tin
null
c1ccsc1.c1cncnc1
c1cncnc1.c1ccsc1
c1cncnc1.c1ccsc1
HBr.Sn
null
null
null
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1ccsc1.Clc1ncc(Br)cn1>>Clc1ncc(-c2ccsc2)cn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-271624f9843942ab8442a38e02129aa7
ClCc1ccsc1.Oc1cnc(Cl)nc1>>Clc1ncc(OCc2ccsc2)cn1
ClC1=NC=C(C=N1)O.ClCC1=CSC=C1.C([O-])([O-])=O.[K+].[K+].CN(C=O)C>>ClC1=NC=C(C=N1)OCC1=CSC=C1
Cl[CH2:7][c:8]1[cH:9][cH:10][s:11][cH:12]1.[Cl:1][c:2]1[n:3][cH:4][c:5]([OH:6])[cH:13][n:14]1>>[Cl:1][c:2]1[n:3][cH:4][c:5]([O:6][CH2:7][c:8]2[cH:9][cH:10][s:11][cH:12]2)[cH:13][n:14]1
ClCc1ccsc1.Oc1cnc(Cl)nc1
Clc1ncc(OCc2ccsc2)cn1
null
null
O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
c1ncc(OCc2ccsc2)cn1
Cl-[CH2;D2;+0:1]-[c:2]1:[c:3]:[#16;a:4]:[c:5]:[c:6]:1.[OH;D1;+0:7]-[c:8]1:[c:9]:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:1>>[#16;a:4]1:[c:5]:[c:6]:[c:2](-[CH2;D2;+0:1]-[O;H0;D2;+0:7]-[c:8]2:[c:9]:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:2):[c:3]:1
99.3
[{"value": 99.3, "product": "ClC1=NC=C(C=N1)OCC1=CSC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
1
HOUR
A mixture of 2-chloro-5-hydroxypyrimidine (200 mg), 3-chloromethylthiophene (610 mg), potassium carbonate (635 mg) and dimethylformamide (3 ml) is stirred at 50° C. for one hour. After the reaction is complete, to the reaction mixture is added water, and extracted with ethyl acetate. The organic layer is washed with wa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1cncnc1.c1ccsc1
HCl
O
50
1
ClCc1ccsc1.Oc1cnc(Cl)nc1>O>Clc1ncc(OCc2ccsc2)cn1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-202ad24f23144e29a486e05cf3ccb4db
NC(=O)c1cc(N)ccc1C(=O)Nc1ccc(N)cc1>>N#Cc1cc(N)ccc1C(=O)Nc1ccc(N)cc1
CC(=O)C.OS(=O)(=O)O.O=S(=O)=O.NC1=CC=C(C(=O)NC2=CC=C(C=C2)N)C(=C1)C(N)=O.[NH4+].[OH-]>>NC1=CC=C(C(=O)NC2=CC=C(C=C2)N)C(=C1)C#N
O=[C:2]([NH2:1])[c:3]1[cH:4][c:5]([NH2:6])[cH:7][cH:8][c:9]1[C:10](=[O:11])[NH:12][c:13]1[cH:14][cH:15][c:16]([NH2:17])[cH:18][cH:19]1>>[N:1]#[C:2][c:3]1[cH:4][c:5]([NH2:6])[cH:7][cH:8][c:9]1[C:10](=[O:11])[NH:12][c:13]1[cH:14][cH:15][c:16]([NH2:17])[cH:18][cH:19]1
NC(=O)c1cc(N)ccc1C(=O)Nc1ccc(N)cc1
N#Cc1cc(N)ccc1C(=O)Nc1ccc(N)cc1
null
null
C(C)O
Miscellaneous
OtherReaction
5094e9d814705bbdc421edbf7e9198e499e70e93916e2cec6eefbc82d1ba5440
32b9893bcb5223559a9d02852f8392cf6473aacfb044a52ba4e9cb9c29edb170
O=C(Nc1ccccc1)c1ccccc1
O=[C;H0;D3;+0:1](-[NH2;D1;+0:2])-[c:3](:[c:4]):[c:5]-[C:6](-[#7:7])=[O;D1;H0:8]>>[#7:7]-[C:6](=[O;D1;H0:8])-[c:5]:[c:3](-[C;H0;D2;+0:1]#[N;H0;D1;+0:2]):[c:4]
null
[]
null
null
null
null
350 ml of oleum (30% by weight) was cooled down below 0° C. using an ice bath, 99.6 g (0.368 mol) of 4,4'-diamino-6-carbamoyl benzanilide in a powder form was added below 5° C. with stirring. The stirring was continued to the next day, and the solution was neutralized by adding 1100 ml of NH4OH (28% by weight) already ...
10.6084/m9.figshare.5104873.v1
null
Primary amide
Nitrile
null
null
c1ccccc1.c1ccccc1
HO-
C(C)O
null
null
NC(=O)c1cc(N)ccc1C(=O)Nc1ccc(N)cc1>C(C)O>N#Cc1cc(N)ccc1C(=O)Nc1ccc(N)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b9cf0611d38749c6a169a2037a147be6
C1CCOC1.O=C1N[C@H](c2ccccc2)CO1>>CCCC[N+](CCCC)(CCCC)CCCC.O=C1N[C@H](c2ccccc2)CO1
C1(=CC=CC=C1)[C@H]1NC(OC1)=O.[H-].[Na+].C1CCOC1>>C(CCC)[N+](CCCC)(CCCC)CCCC.C1(=CC=CC=C1)[C@H]1NC(OC1)=O
O1[CH2:1][CH2:14][CH2:15][CH2:16]1.[NH:5]1[C:19](=[O:18])[O:29][CH2:28][C@H:21]1[c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[CH3:1][CH2:2][CH2:3][CH2:4][N+:5]([CH2:6][CH2:7][CH2:8][CH3:9])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:14][CH2:15][CH2:16][CH3:17].[O:18]=[C:19]1[NH:20][C@H:21]([c:22]2[cH:23][cH:24][cH:25][cH:26...
C1CCOC1.O=C1N[C@H](c2ccccc2)CO1
CCCC[N+](CCCC)(CCCC)CCCC.O=C1N[C@H](c2ccccc2)CO1
null
[Br-].C(CCC)[N+](CCCC)(CCCC)CCCC
null
C-C Coupling
OtherReaction
09778d9af7fde04154af0e39592ee4ce448955ccce539b65b1ac70ac1566a02b
c65c4f96eb20735d6c3621ff639a0b1b80493ea2862415b9e2d7a24c0b0536a0
O=C1N[C@H](c2ccccc2)CO1
O1-[CH2;D2;+0:1]-[C:2]-[CH2;D2;+0:3]-[CH2;D2;+0:4]-1.[O;D1;H0:5]=[C;H0;D3;+0:6]1-[#8:7]-[C:8]-[C@@H;D3;+0:9](-[c:10](:[c:11]):[c:12])-[NH;D2;+0:13]-1>>[C:14]-[C:15]-[N+;H0;D4:13](-[C:16]-[C:17]-[C:18]-[CH3;D1;+0:4])(-[C:19]-[C:20])-[CH2;D2;+0:3]-[C:2]-[CH2;D2;+0:1]-[C;D1;H3:21].[O;D1;H0:5]=[C;H0;D3;+0:6]1-[#7:22]-[C@H;...
null
[]
null
null
30
MINUTE
To a stirred solution of (R)-4-phenyl-2-oxazolidinone (174 mg, 1.06 mmol) in THF (4 mL) at 0° C., add NaH (4.3 mg, 60% emulsion in oil, 0.106 mmol). Allow the temperature to rise to room temperature over 30 min., then add tetra n-butylammonium bromide (34 mg, 0.106 mmol) to the mixture and stir for another 30 min. to o...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether
Carbamic ester.Ether
C1CCOC1.C1COCN1
C1COCN1
C1COCN1.c1ccccc1
null
[Br-].C(CCC)[N+](CCCC)(CCCC)CCCC
null
0.5
C1CCOC1.O=C1N[C@H](c2ccccc2)CO1>[Br-].C(CCC)[N+](CCCC)(CCCC)CCCC>CCCC[N+](CCCC)(CCCC)CCCC.O=C1N[C@H](c2ccccc2)CO1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-76651472f2d84918bce8909e6a061689
Clc1ccc(I)cc1.Clc1ccccc1Cl.c1ccc(Nc2ccc(Nc3ccccc3)cc2)cc1>>Clc1ccc(N(c2ccccc2)c2ccc(N(c3ccccc3)c3ccc(Cl)cc3)cc2)cc1
C1(=CC=CC=C1)NC1=CC=C(C=C1)NC1=CC=CC=C1.IC1=CC=C(C=C1)Cl.C1COCCOCCOCCOCCOCCO1.C([O-])([O-])=O.[K+].[K+].ClC1=C(C=CC=C1)Cl>>C1(=CC=CC=C1)N(C1=CC=C(C=C1)N(C1=CC=C(C=C1)Cl)C1=CC=CC=C1)C1=CC=C(C=C1)Cl
I[c:5]1[cH:4][cH:3][c:2]([Cl:1])[cH:34][cH:33]1.Cl[c:23]1[c:18]([Cl:28])[cH:19][cH:20][cH:21][cH:22]1.[NH:6]([c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1)[c:13]1[cH:14][cH:15][c:16]([NH:17][c:24]2[cH:25][cH:26][cH:27][cH:29][cH:30]2)[cH:31][cH:32]1>>[Cl:1][c:2]1[cH:3][cH:4][c:5]([N:6]([c:7]2[cH:8][cH:9][cH:10][cH:11][cH:12...
Clc1ccc(I)cc1.Clc1ccccc1Cl.c1ccc(Nc2ccc(Nc3ccccc3)cc2)cc1
Clc1ccc(N(c2ccccc2)c2ccc(N(c3ccccc3)c3ccc(Cl)cc3)cc2)cc1
null
[Cu]
CCCCCC.C(Cl)Cl
Heteroatom Alkylation and Arylation
OtherReaction
a653c775af516c3ff5ab1e2464b502a5e949e2df9114685330a6fec3418ed0b4
f418d6272dad02aa82458c3dd91cd15bb8781bb54b86d001423e443c7ae41e4e
c1ccc(N(c2ccccc2)c2ccc(N(c3ccccc3)c3ccccc3)cc2)cc1
Cl-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[c:5]:[c;H0;D3;+0:6]:1-[Cl;H0;D1;+0:7].I-[c;H0;D3;+0:8](:[c:9]:[c:10]):[c:11]:[c:12].[c:13]:[c:14](-[NH;D2;+0:15]-[c:16]1:[c:17]:[c:18]:[c:19](-[NH;D2;+0:20]-[c:21]2:[c:22]:[c:23]:[cH;D2;+0:24]:[c:25]:[c:26]:2):[c:27]:[c:28]:1):[c:29]>>[Cl;H0;D1;+0:7]-[c;H0;D3;+0:24]1:[c:23]:[c:22]:...
null
[]
200
CELSIUS
null
null
A 1 L, three-necked, round-bottomed flask, equipped with an overhead stirrer, a nitrogen inlet and a reflux condenser, was charged with N,N'-diphenyl-1,4-phenylenediamine (13.0 g, 0.05 mol), 4-iodochlorobenzene (31.0 g, 0.13 mol), copper bronze powder (12.7 g, 0.20 mol), 18-crown-6 ether (2.6 g, 0.10 mol), powdered pot...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic halide.Aromatic halide.Secondary amine.Secondary amine
Aromatic halide.Tertiary amine.Tertiary amine
c1ccccc1.c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
HCl.I-
[Cu].CCCCCC.C(Cl)Cl
200
null
Clc1ccc(I)cc1.Clc1ccccc1Cl.c1ccc(Nc2ccc(Nc3ccccc3)cc2)cc1>[Cu].CCCCCC.C(Cl)Cl>Clc1ccc(N(c2ccccc2)c2ccc(N(c3ccccc3)c3ccc(Cl)cc3)cc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ec0108d9114945ba9e887e8acb30ed7f
NC(=O)Nc1ccccc1.NN>>NNC(=O)Nc1ccccc1
NN.C1(=CC=CC=C1)NC(=O)N.NN>>C1(=CC=CC=C1)NC(NN)=O
[NH2:2][C:3](=[O:4])[NH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1.N[NH2:1]>>[NH2:1][NH:2][C:3](=[O:4])[NH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1
NC(=O)Nc1ccccc1.NN
NNC(=O)Nc1ccccc1
null
null
null
Miscellaneous
OtherReaction
e1c7dc7a5e70fef253b7e7f40a6385158a3c16d71bafa884450868de51a521b9
29efa48fb47552659a572494b97672efdaf1b6ae73a63009d32288dec9b93edb
c1ccccc1
N-[NH2;D1;+0:1].[NH2;D1;+0:2]-[C:3](=[O;D1;H0:4])-[#7:5]-[c:6]>>[NH2;D1;+0:1]-[NH;D2;+0:2]-[C:3](=[O;D1;H0:4])-[#7:5]-[c:6]
null
[]
null
null
null
null
Other known methods for the preparation of 4-aryl-1,2,4-triazol-3-ones involve the use of hydrazine as a raw material. In one such method, phenylurea is reacted with hydrazine to give a 4-phenylsemicarbazide. The semicarbazide is then condensed with ethyl formate to give the 4-phenyltriazolone. The overall yield from t...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Urea
Acylhydrazine
null
null
c1ccccc1
Other
null
null
null
NC(=O)Nc1ccccc1.NN>>NNC(=O)Nc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e99cd70b8d1c4b8eabefb6d92273d488
NNC(=O)Nc1ccccc1.O=CO>>O=CNNC(=O)Nc1ccccc1
C1(=CC=CC=C1)NC(NN)=O.C(=O)O>>C(=O)NNC(=O)NC1=CC=CC=C1
[NH2:3][NH:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1.O[CH:2]=[O:1]>>[O:1]=[CH:2][NH:3][NH:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][cH:10][cH:11][cH:12][cH:13]1
NNC(=O)Nc1ccccc1.O=CO
O=CNNC(=O)Nc1ccccc1
null
null
null
Acylation
Carboxylic acid with primary amine to amide
1bfc5046b360bb38c235d234cdd252f03d34a0792ef57a2cdb032482310d9689
1f93e2b4a6ed796a4645f0486672499ca332a9bc5c180e504c9a46d8eb8d844d
c1ccccc1
O-[CH;D2;+0:1]=[O;D1;H0:2].[#7:3]-[C:4](=[O;D1;H0:5])-[#7:6]-[NH2;D1;+0:7]>>[#7:3]-[C:4](=[O;D1;H0:5])-[#7:6]-[NH;D2;+0:7]-[CH;D2;+0:1]=[O;D1;H0:2]
null
[]
null
null
null
null
Other known methods for the preparation of 4-aryl-1,2,4-triazol-3-ones involve the use of hydrazine as a raw material. In one such method, phenylurea is reacted with hydrazine to give a 4-phenylsemicarbazide. The semicarbazide is then condensed with ethyl formate to give the 4-phenyltriazolone. The overall yield from t...
10.6084/m9.figshare.5104873.v1
null
Acylhydrazine.Carboxylic acid
Acylhydrazine.Acylhydrazine
null
null
c1ccccc1
HO-
null
null
null
NNC(=O)Nc1ccccc1.O=CO>>O=CNNC(=O)Nc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c607dee34d244a7e8f565c496317fb94
FC(F)=CCCBr.Sc1nc2ccccc2s1>>FC(F)=CCCSc1nc2ccccc2s1
BrCCC=C(F)F.BrCCC=C(F)F.C([O-])([O-])=O.[K+].[K+].SC=1SC2=C(N1)C=CC=C2.C([O-])([O-])=O.[K+].[K+]>>FC(=CCCSC=1SC2=C(N1)C=CC=C2)F
Br[CH2:6][CH2:5][CH:4]=[C:2]([F:1])[F:3].[SH:7][c:8]1[n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[s:16]1>>[F:1][C:2]([F:3])=[CH:4][CH2:5][CH2:6][S:7][c:8]1[n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[s:16]1
FC(F)=CCCBr.Sc1nc2ccccc2s1
FC(F)=CCCSc1nc2ccccc2s1
null
null
ClCCl
Heteroatom Alkylation and Arylation
thioether_nucl_sub
26df88c6a3f5f203c89584658be4e126cb42994c98a2e16bc812e1036cdae857
8b2f52296c3a93039174c980b6042ba15754e04d6892a1284c3a32985220b214
c1ccc2scnc2c1
Br-[CH2;D2;+0:1]-[C:2]-[C:3]=[C:4](-[F;D1;H0:5])-[F;D1;H0:6].[SH;D1;+0:7]-[c:8]1:[#16;a:9]:[c:10]:[c:11]:[#7;a:12]:1>>[F;D1;H0:5]-[C:4](-[F;D1;H0:6])=[C:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:7]-[c:8]1:[#16;a:9]:[c:10]:[c:11]:[#7;a:12]:1
63
[{"value": 63.0, "product": "FC(=CCCSC=1SC2=C(N1)C=CC=C2)F", "details": "PERCENTYIELD", "is_desired": false}]
55
CELSIUS
6
HOUR
To the solution of 4-bromo-1,1-difluorobut-1-ene prepared in Example 6 was added potassium carbonate (10.76 g) and 2-mercaptobenzthiazole (9.18 g). The mixture was stirred at 55° C. for 6 hours and then at room temperature overnight. Gas-liquid chromatography of a sample of the reaction mixture showed that a small amou...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic thiol
Monosulfide
null
null
c1ccc2scnc2c1
HBr
ClCCl
55
6
FC(F)=CCCBr.Sc1nc2ccccc2s1>ClCCl>FC(F)=CCCSc1nc2ccccc2s1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2e60c0ccb53946718e5945e7423510f1
FC(CCBr)C(F)(F)Br.Sc1nc2ccccc2o1>>FC(F)=CCCSc1nc2ccccc2o1
BrC(C(CCBr)F)(F)F.SC=1OC2=C(N1)C=CC=C2>>FC(=CCCSC=1OC2=C(N1)C=CC=C2)F
F[CH:4]([C:2](Br)([F:1])[F:3])[CH2:5][CH2:6]Br.[SH:7][c:8]1[n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[o:16]1>>[F:1][C:2]([F:3])=[CH:4][CH2:5][CH2:6][S:7][c:8]1[n:9][c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[o:16]1
FC(CCBr)C(F)(F)Br.Sc1nc2ccccc2o1
FC(F)=CCCSc1nc2ccccc2o1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3cdc643e2774edc9dd189ce32ffd0fa7797615837737c802aea81ea08103e059
cb2f0132bcb1bf39bd4ac1f7bebbd736b8da28ab9cc03a2c62b248ebd3ed904b
c1ccc2ocnc2c1
Br-[CH2;D2;+0:1]-[C:2]-[CH;D3;+0:3](-F)-[C;H0;D4;+0:4](-Br)(-[F;D1;H0:5])-[F;D1;H0:6].[SH;D1;+0:7]-[c:8]1:[#7;a:9]:[c:10]:[c:11]:[#8;a:12]:1>>[F;D1;H0:5]-[C;H0;D3;+0:4](-[F;D1;H0:6])=[CH;D2;+0:3]-[C:2]-[CH2;D2;+0:1]-[S;H0;D2;+0:7]-[c:8]1:[#7;a:9]:[c:10]:[c:11]:[#8;a:12]:1
null
[]
null
null
null
null
To the solution of 4-bromo-1,1-difluorobut-1-ene prepared in Example 6 was added potassium carbonate (10.76 g) and 2-mercaptobenzthiazole (9.18 g). The mixture was stirred at 55° C. for 6 hours and then at room temperature overnight. Gas-liquid chromatography of a sample of the reaction mixture showed that a small amou...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Tertiary halide.Tertiary halide.Secondary halide.Primary halide.Aromatic thiol
Alkenyl halide.Alkenyl halide.Monosulfide
null
null
c1ccc2ocnc2c1
HF.Br-
null
null
null
FC(CCBr)C(F)(F)Br.Sc1nc2ccccc2o1>>FC(F)=CCCSc1nc2ccccc2o1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-640b83ec08f243538919c6f734081f30
C[Si](C)(C)CCOCn1nccc1C(=O)c1ccccc1[N+](=O)[O-]>>C[Si](C)(C)CCOCn1nccc1C(=O)c1ccccc1N
[N+](=O)([O-])C1=C(C(=O)C2=CC=NN2COCC[Si](C)(C)C)C=CC=C1>>NC1=C(C(=O)C2=CC=NN2COCC[Si](C)(C)C)C=CC=C1
O=[N+:22]([O-])[c:21]1[c:16]([C:14]([c:13]2[n:9]([CH2:8][O:7][CH2:6][CH2:5][Si:2]([CH3:1])([CH3:3])[CH3:4])[n:10][cH:11][cH:12]2)=[O:15])[cH:17][cH:18][cH:19][cH:20]1>>[CH3:1][Si:2]([CH3:3])([CH3:4])[CH2:5][CH2:6][O:7][CH2:8][n:9]1[n:10][cH:11][cH:12][c:13]1[C:14](=[O:15])[c:16]1[cH:17][cH:18][cH:19][cH:20][c:21]1[NH2:...
C[Si](C)(C)CCOCn1nccc1C(=O)c1ccccc1[N+](=O)[O-]
C[Si](C)(C)CCOCn1nccc1C(=O)c1ccccc1N
null
null
C1CCOC1
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C(c1ccccc1)c1ccn[nH]1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]-[C:5]=[O;D1;H0:6]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]-[C:5]=[O;D1;H0:6]
49
[{"value": 49.0, "product": "NC1=C(C(=O)C2=CC=NN2COCC[Si](C)(C)C)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 48.8, "product": "NC1=C(C(=O)C2=CC=NN2COCC[Si](C)(C)C)C=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
The mixture of pyrazoles of examples 13C and 13D (2.35 g, 6.772 mmol) was taken up in dry THF (100 ml) and degassed. 5% Pd.-on-carbon (1.2 g) was added and the mixture hydrogenated at 30 psi and ambient temperature for 2 h. The mixture was filtered (celite filter aid) and evaporated and then chromatographed (eluant 30%...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccn[nH]1.c1ccccc1
Other
C1CCOC1
null
2
C[Si](C)(C)CCOCn1nccc1C(=O)c1ccccc1[N+](=O)[O-]>C1CCOC1>C[Si](C)(C)CCOCn1nccc1C(=O)c1ccccc1N
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-39eb4353217146abafbc990f86f0185c
CCOC(=O)NC1N=C(c2ccccn2)c2ccccc2N(CC(=O)C(C)(C)C)C1=O>>CC(C)(C)C(=O)CN1C(=O)C(N)N=C(c2ccccn2)c2ccccc21
C(C)OC(=O)NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O.Br>>NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O
CCOC(=O)[NH:12][CH:11]1[C:9](=[O:10])[N:8]([CH2:7][C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[O:6])[c:26]2[c:21]([cH:22][cH:23][cH:24][cH:25]2)[C:14]([c:15]2[cH:16][cH:17][cH:18][cH:19][n:20]2)=[N:13]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[CH2:7][N:8]1[C:9](=[O:10])[CH:11]([NH2:12])[N:13]=[C:14]([c:15]2[cH:16][cH:17]...
CCOC(=O)NC1N=C(c2ccccn2)c2ccccc2N(CC(=O)C(C)(C)C)C1=O
CC(C)(C)C(=O)CN1C(=O)C(N)N=C(c2ccccn2)c2ccccc21
null
null
C(Cl)Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
878b485764081f6281e68f2ba6bab7d31c31c0c91b0b8d3614e74f76907da827
4e549866ec1acadec4c84aaf8495992a28ec78d8ea5ef1b9f44dd843b0dcb7d4
O=C1CN=C(c2ccccn2)c2ccccc2N1
C-C-O-C(=O)-[NH;D2;+0:1]-[C:2](-[#7:3]=[C:4])-[C:5](=[O;D1;H0:6])-[#7:7](-[C:8]-[C:9]=[O;D1;H0:10])-[c:11]>>[C:4]=[#7:3]-[C:2](-[NH2;D1;+0:1])-[C:5](=[O;D1;H0:6])-[#7:7](-[C:8]-[C:9]=[O;D1;H0:10])-[c:11]
91
[{"value": 91.0, "product": "NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.6, "product": "NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
64
HOUR
(3RS)-Ethyloxycarbonylamino-1-(tert-butylcarbonylmethyl)-2,3-dihydro-5-(2-pyridyl)-1H-1,4-benzodiazepin-2-one (IV, 250 mg, 0.592 mmol) was taken up in dry DCM (10 ml) at 0° C. and saturated with dry HBr gas. The mixture was stoppered and stirred at r.t. for 64 h. The solvent was evaporated and the product partitioned b...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether
Primary amine
null
null
c1ccncc1.C1=NCC[NH]c2ccccc21
HO-
C(Cl)Cl
null
64
CCOC(=O)NC1N=C(c2ccccn2)c2ccccc2N(CC(=O)C(C)(C)C)C1=O>C(Cl)Cl>CC(C)(C)C(=O)CN1C(=O)C(N)N=C(c2ccccn2)c2ccccc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5570e335404a45e8bde112385306c6b2
Nc1cccc(C(=O)O)c1.O=CO>>O=CNc1cccc(C(=O)O)c1
C(C)(=O)OC(C)=O.C(=O)O.NC=1C=C(C(=O)O)C=CC1>>C(=O)NC=1C=C(C(=O)O)C=CC1
[NH2:3][c:4]1[cH:5][cH:6][cH:7][c:8]([C:9](=[O:10])[OH:11])[cH:12]1.O[CH:2]=[O:1]>>[O:1]=[CH:2][NH:3][c:4]1[cH:5][cH:6][cH:7][c:8]([C:9](=[O:10])[OH:11])[cH:12]1
Nc1cccc(C(=O)O)c1.O=CO
O=CNc1cccc(C(=O)O)c1
null
null
O
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccccc1
O-[CH;D2;+0:1]=[O;D1;H0:2].[NH2;D1;+0:3]-[c:4](:[c:5]):[c:6]>>[O;D1;H0:2]=[CH;D2;+0:1]-[NH;D2;+0:3]-[c:4](:[c:5]):[c:6]
null
[]
null
null
null
null
Acetic anhydride (76 ml) was added to 98% formic acid (130 ml) and the mixture stirred at r.t. 30 min, then 3-aminobenzoic acid (15 g, 109.5 mmol) added. The mixture was stirred at r.t. for 1 h, then water (1.3 L) added and stirring continued overnight. The resultant white precipitate was collected, washed with water a...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1
HO-
O
null
null
Nc1cccc(C(=O)O)c1.O=CO>O>O=CNc1cccc(C(=O)O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a5a2655fdf3f4f1cbc09910d0b12df9c
CI.O=CNc1cccc(C(=O)O)c1>>CN(C=O)c1ccccc1C(=O)O
IC.CN(C)C=O.C(=O)NC=1C=C(C(=O)O)C=CC1.[H-].[Na+].CN(C)C=O.IC>>C(=O)N(C)C1=C(C(=O)O)C=CC=C1
I[CH3:1].[NH:2]([CH:3]=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:10]([C:11](=[O:12])[OH:13])[cH:9]1>>[CH3:1][N:2]([CH:3]=[O:4])[c:5]1[cH:6][cH:7][cH:8][cH:9][c:10]1[C:11](=[O:12])[OH:13]
CI.O=CNc1cccc(C(=O)O)c1
CN(C=O)c1ccccc1C(=O)O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
c9d83082ec710521e15304c050f42d0f8122726753293668018fe69df2107ba0
0a16658309ac5595448433dd7ef49294830b145345df0b202ccd54727262e629
c1ccccc1
I-[CH3;D1;+0:1].[O;D1;H0:2]=[C:3](-[O;D1;H1:4])-[c;H0;D3;+0:5]1:[cH;D2;+0:6]:[c:7]:[c:8]:[c;H0;D3;+0:9](-[NH;D2;+0:10]-[C:11]=[O;D1;H0:12]):[cH;D2;+0:13]:1>>[CH3;D1;+0:1]-[N;H0;D3;+0:10](-[C:11]=[O;D1;H0:12])-[c;H0;D3;+0:9]1:[c:8]:[c:7]:[cH;D2;+0:6]:[cH;D2;+0:13]:[c;H0;D3;+0:5]:1-[C:3](=[O;D1;H0:2])-[O;D1;H1:4]
86
[{"value": 86.0, "product": "C(=O)N(C)C1=C(C(=O)O)C=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
3-Formylamino benzoic acid (2.28 g, 13.8 mmol) was taken up in DMF (25 ml) and added dropwise to a suspension of sodium hydride (1.05 g, 80% disp. in oil) in DMF (15 ml) at 0° C. The mixture was allowed to warm to r.t. over 1 h and then iodomethane (0.95 ml) added. A second portion of iodomethane (0.95 ml) was added af...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Tertiary amide
c1ccccc1
c1ccccc1
c1ccccc1
HI
null
null
8
CI.O=CNc1cccc(C(=O)O)c1>>CN(C=O)c1ccccc1C(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-21d973d5e9c342b28599ca4532af6af7
C=CCCC(=O)Cl.COC(=O)c1cccc(N)c1>>C=CCCC(=O)Nc1cccc(C(=O)OC)c1
COC(C1=CC(=CC=C1)N)=O.C(CCC=C)(=O)Cl.C(CCC=C)(=O)O.S(=O)(Cl)Cl>>C(CCC=C)(=O)NC=1C=C(C(=O)OC)C=CC1
Cl[C:5]([CH2:4][CH2:3][CH:2]=[CH2:1])=[O:6].[NH2:7][c:8]1[cH:9][cH:10][cH:11][c:12]([C:13](=[O:14])[O:15][CH3:16])[cH:17]1>>[CH2:1]=[CH:2][CH2:3][CH2:4][C:5](=[O:6])[NH:7][c:8]1[cH:9][cH:10][cH:11][c:12]([C:13](=[O:14])[O:15][CH3:16])[cH:17]1
C=CCCC(=O)Cl.COC(=O)c1cccc(N)c1
C=CCCC(=O)Nc1cccc(C(=O)OC)c1
null
null
C(Cl)Cl.N1=CC=CC=C1
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
c1ccccc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]-[C:5]=[C;D1;H2:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[C;D1;H2:6]=[C:5]-[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10]
32
[{"value": 32.0, "product": "C(CCC=C)(=O)NC=1C=C(C(=O)OC)C=CC1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
Methyl(3-amino)benzoate (4.5 g, 29.8 mmol) was taken up in DCM (10 ml) and pyridine (1 ml) at 0° C. 4-Pentenoyl chloride (freshly prepared from 4-pentenoic acid (3.0 g, 29.97 mmol) and thionyl chloride (6.6 ml) at r.t. for 1 h, evaporated and azeotroped with DCM) was added dropwise in DCM (3 ml). The mixture was allowe...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccccc1
HCl
C(Cl)Cl.N1=CC=CC=C1
null
8
C=CCCC(=O)Cl.COC(=O)c1cccc(N)c1>C(Cl)Cl.N1=CC=CC=C1>C=CCCC(=O)Nc1cccc(C(=O)OC)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-39e2a12366cc4afaa1054c2e96602afd
COC(=O)c1cccc(NC(=O)CCCCBr)c1>>COC(=O)c1cccc(N2CCCCC2=O)c1
BrCCCCC(=O)NC=1C=C(C(=O)OC)C=CC1.[H-].[Na+]>>O=C1N(CCCC1)C=1C=C(C(=O)OC)C=CC1
Br[CH2:11][CH2:12][CH2:13][CH2:14][C:15]([NH:10][c:9]1[cH:8][cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:17]1)=[O:16]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][CH2:13][CH2:14][C:15]2=[O:16])[cH:17]1
COC(=O)c1cccc(NC(=O)CCCCBr)c1
COC(=O)c1cccc(N2CCCCC2=O)c1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
9dfd2b7906d79dea91b8c168207af33ec48cc64e1e8d843c068b11dc21f26e62
4a6c1e88c9e8bed487b746792f88d478ff36cc235f9a217d4632e6babdebdc9a
O=C1CCCCN1c1ccccc1
Br-[CH2;D2;+0:1]-[C:2]-[C:3]-[C:4]-[C:5](=[O;D1;H0:6])-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10]>>[O;D1;H0:6]=[C:5]1-[C:4]-[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:7]-1-[c:8](:[c:9]):[c:10]
56.2
[{"value": 56.0, "product": "O=C1N(CCCC1)C=1C=C(C(=O)OC)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 56.2, "product": "O=C1N(CCCC1)C=1C=C(C(=O)OC)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
The bromide of Example 36 (1.50 g, 4.88 mmol) was taken up in dry DMF (40 ml) and treated with NaH (160 mg, 80% disp. in oil) at 0° C. The mixture was stirred at r.t. under nitrogen for 10 min, then KI (80 mg) added and the mixture heated at 70° C. for 4 h. The mixture was evaporated and partitioned between EtOAc and 1...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amide
Tertiary amide
null
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1
HBr
CN(C)C=O
null
0.166667
COC(=O)c1cccc(NC(=O)CCCCBr)c1>CN(C)C=O>COC(=O)c1cccc(N2CCCCC2=O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b2a2fb45af4f44099c49615f8d09865c
COC(=O)c1cccc(N2CCCCC2=O)c1>>COC(=O)c1cccc(N2CCCCC2)c1
O=C1N(CCCC1)C=1C=C(C(=O)OC)C=CC1.B.O1CCCC1>>N1(CCCCC1)C=1C=C(C(=O)OC)C=CC1
O=[C:15]1[N:10]([c:9]2[cH:8][cH:7][cH:6][c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:16]2)[CH2:11][CH2:12][CH2:13][CH2:14]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:9]([N:10]2[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]2)[cH:16]1
COC(=O)c1cccc(N2CCCCC2=O)c1
COC(=O)c1cccc(N2CCCCC2)c1
null
null
C1CCOC1
Reduction
Reduction of tertiary amides to amines
a9fd579e7faaaa094227b38014f5494172546cdc7c9d2d1b8815d615c0aa21f2
c8f3c617792f7a4fae96b8a97dc0ce23461ab85d8a738fe6caacff776ef51ffa
c1ccc(N2CCCCC2)cc1
O=[C;H0;D3;+0:1](-[C:2]-[C:3])-[#7:4](-[c:5])-[C:6]>>[C:6]-[#7:4](-[c:5])-[CH2;D2;+0:1]-[C:2]-[C:3]
90
[{"value": 90.0, "product": "N1(CCCCC1)C=1C=C(C(=O)OC)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.5, "product": "N1(CCCCC1)C=1C=C(C(=O)OC)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
The compound of Example 37 (640 mg, 2.75 mmol) was dissolved in dry THF (30 ml) and borane-tetrahydrofuran complex (5 ml, 1M solution in THF) was added. The mixture was stirred under nitrogen under reflux for 1 h, then cooled and evaporated. The residue was taken up in MeOH/acetic acid (6/1, v/v, 70 ml) and heated unde...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide
null
C1CC[NH]CC1
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1
Other
C1CCOC1
null
null
COC(=O)c1cccc(N2CCCCC2=O)c1>C1CCOC1>COC(=O)c1cccc(N2CCCCC2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-227139b0204b412c8ef4f1e745340ffc
COC(=O)c1cccc(N2CCCCC2)c1>>O=C(O)c1cccc(N2CCCCC2)c1
N1(CCCCC1)C=1C=C(C(=O)OC)C=CC1.O.[OH-].[Li+].C(C)(=O)O>>N1(CCCCC1)C=1C=C(C(=O)O)C=CC1
C[O:3][C:2](=[O:1])[c:4]1[cH:5][cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]2)[cH:15]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][cH:7][c:8]([N:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]2)[cH:15]1
COC(=O)c1cccc(N2CCCCC2)c1
O=C(O)c1cccc(N2CCCCC2)c1
null
null
O.O1CCOCC1
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(N2CCCCC2)cc1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4]
90
[{"value": 90.0, "product": "N1(CCCCC1)C=1C=C(C(=O)O)C=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 88.9, "product": "N1(CCCCC1)C=1C=C(C(=O)O)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
40
CELSIUS
1
HOUR
The compound of Example 38 (540 mg, 2.466 mmol) was dissolved in dioxan (12 ml) and water (8 ml). Lithium hydroxide hydrate (300 mg, 7.143 mmol) was added and the mixture stirred at 40° C. for 1 h. The mixture was acidified with acetic acid, evaporated, azeotroped with toluene and chromatographed on silica (eluant 60/4...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.C1CC[NH]CC1
Other
O.O1CCOCC1
40
1
COC(=O)c1cccc(N2CCCCC2)c1>O.O1CCOCC1>O=C(O)c1cccc(N2CCCCC2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5df61b0f843d454b91abd7c3ea08a12b
CCOC(N)=O.O=CC(=O)O.c1ccc2[nH]nnc2c1>>CCOC(=O)N(CC(=O)O)n1nnc2ccccc21
C(N)(OCC)=O.O.C(C=O)(=O)O.N1N=NC2=C1C=CC=C2>>C(C)OC(=O)N(CC(=O)O)N1N=NC2=C1C=CC=C2
[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH2:6].O=[CH:7][C:8](=[O:9])[OH:10].[nH:11]1[n:12][n:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]12>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[N:6]([CH2:7][C:8](=[O:9])[OH:10])[n:11]1[n:12][n:13][c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]12
CCOC(N)=O.O=CC(=O)O.c1ccc2[nH]nnc2c1
CCOC(=O)N(CC(=O)O)n1nnc2ccccc21
null
null
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
OtherReaction
f2955afb7a3443f2b2c397c64400d5c18b12961d9a2e873e83477c7c17c5b083
75f6f3cbd3c0325a929f41a15c9cdeffc50914512b22e7019b0acebcd00ef2c9
c1ccc2[nH]nnc2c1
O=[CH;D2;+0:1]-[C:2](=[O;D1;H0:3])-[O;D1;H1:4].[C:5]-[#8:6]-[C:7](-[NH2;D1;+0:8])=[O;D1;H0:9].[c:10]:[c:11]1:[#7;a:12]:[#7;a:13]:[nH;D2;+0:14]:[c:15]:1:[c:16]>>[C:5]-[#8:6]-[C:7](=[O;D1;H0:9])-[N;H0;D3;+0:8](-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[O;D1;H1:4])-[n;H0;D3;+0:14]1:[#7;a:13]:[#7;a:12]:[c:11](:[c:10]):[c:15]:1:[c...
96
[{"value": 96.0, "product": "C(C)OC(=O)N(CC(=O)O)N1N=NC2=C1C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.8, "product": "C(C)OC(=O)N(CC(=O)O)N1N=NC2=C1C=CC=C2", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
15
CELSIUS
8
HOUR
Ethyl carbamate (69.0 g, 774.5 mmol), glyoxylic acid hydrate (71.3 g, 774.5 mmol) and benzotriazole (92.0 g, 774.5 mmol) were dissolved in toluene (2.3 1) and the mixture was heated with distillation for 3 h to precipitate the product. The mixture was diluted with toluene (totally 2.3 1) and stirred at 15° C. overnight...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Carbamic ester
Carbamic ester
c1ccc2[nH]nnc2c1
c1ccc2[nH]nnc2c1
c1ccc2[nH]nnc2c1
HO-
C1(=CC=CC=C1)C
15
8
CCOC(N)=O.O=CC(=O)O.c1ccc2[nH]nnc2c1>C1(=CC=CC=C1)C>CCOC(=O)N(CC(=O)O)n1nnc2ccccc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ddb2942de49c4b9a90cdb5a3cda50c77
CCOC(=O)NC1N=C(c2ccccn2)c2ccccc2N(CC(=O)C(C)(C)C)C1=O>>CC(C)(C)C(=O)CN1C(=O)C(N)N=C(c2ccccn2)c2ccccc21
C(C)OC(=O)NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O.Cl>>NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O
CCOC(=O)[NH:12][CH:11]1[C:9](=[O:10])[N:8]([CH2:7][C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[O:6])[c:26]2[c:21]([cH:22][cH:23][cH:24][cH:25]2)[C:14]([c:15]2[cH:16][cH:17][cH:18][cH:19][n:20]2)=[N:13]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[C:5](=[O:6])[CH2:7][N:8]1[C:9](=[O:10])[CH:11]([NH2:12])[N:13]=[C:14]([c:15]2[cH:16][cH:17]...
CCOC(=O)NC1N=C(c2ccccn2)c2ccccc2N(CC(=O)C(C)(C)C)C1=O
CC(C)(C)C(=O)CN1C(=O)C(N)N=C(c2ccccn2)c2ccccc21
null
null
C(Cl)Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
878b485764081f6281e68f2ba6bab7d31c31c0c91b0b8d3614e74f76907da827
4e549866ec1acadec4c84aaf8495992a28ec78d8ea5ef1b9f44dd843b0dcb7d4
O=C1CN=C(c2ccccn2)c2ccccc2N1
C-C-O-C(=O)-[NH;D2;+0:1]-[C:2](-[#7:3]=[C:4])-[C:5](=[O;D1;H0:6])-[#7:7](-[C:8]-[C:9]=[O;D1;H0:10])-[c:11]>>[C:4]=[#7:3]-[C:2](-[NH2;D1;+0:1])-[C:5](=[O;D1;H0:6])-[#7:7](-[C:8]-[C:9]=[O;D1;H0:10])-[c:11]
93.3
[{"value": 93.0, "product": "NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 93.3, "product": "NC1C(N(C2=C(C(=N1)C1=NC=CC=C1)C=CC=C2)CC(=O)C(C)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
50
HOUR
A solution of (3RS)-ethoxycarbonylamino-1-(tert-butylcarbonylmethyl)-2,3-dihydro-5-(2-pyridyl)-1H-1,4-benzodiazepin-2-one (10.0 g, 23.7 mmol) in DCM (40 ml) was added to the above solution below 25° C. and the mixture was stirred for 50 h. The mixture was then poured into 3M HCl (80 ml) below 25° C. and the aqueous por...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether
Primary amine
null
null
c1ccncc1.C1=NCC[NH]c2ccccc21
HO-
C(Cl)Cl
null
50
CCOC(=O)NC1N=C(c2ccccn2)c2ccccc2N(CC(=O)C(C)(C)C)C1=O>C(Cl)Cl>CC(C)(C)C(=O)CN1C(=O)C(N)N=C(c2ccccn2)c2ccccc21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-55f511a55d61454a83be8c226edee531
Cl>>Cl
C(C)(C)(C)C(=O)CN1C([C@@H](N=C(C2=C1C=CC=C2)C2=NC=CC=C2)NC(=O)NC2=CC(=CC=C2)N(C)C)=O.C(C)O.Cl>>Cl.C(C)(C)(C)C(=O)CN1C([C@@H](N=C(C2=C1C=CC=C2)C2=NC=CC=C2)NC(=O)NC2=CC(=CC=C2)N(C)C)=O
[ClH:39]>>[ClH:39]
Cl
Cl
null
null
C(C)O
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
50
CELSIUS
8
HOUR
N-((3R)-1-tert-Butylcarbonylmethyl-2,3-dihydro-2-oxo-5-(2-pyridyl)-1H-1,4-benzodiazepin-3-yl)-N'-(3-dimethylaminophenyl)urea (70 g, 136.6 mmol) was taken up in ethanol (1 l) and 2.26M HCl ethanol (63.5 ml, 143.4 mmol) was added dropwise. The mixture was warmed up to 50° C. to afford a clear solution, which was seeded, ...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
C(C)O
50
8
Cl>C(C)O>Cl
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-b0e3813329fd4701a3a3f986ee306d00
CCOC(=O)Cl.CN(C(=O)OC(C)(C)C)c1cccc(C(=O)O)c1>>CN(C(=O)OC(C)(C)C)c1cccc(N=C=O)c1
[N-]=[N+]=[N-].[Na+].CCN(CC)CC.ClC(=O)OCC.O(C(C)(C)C)C(=O)N(C)C=1C=C(C(=O)O)C=CC1>>O(C(C)(C)C)C(=O)N(C)C=1C=C(C=CC1)N=C=O
CCO[C:16](Cl)=[O:17].O=C(O)[c:14]1[cH:13][cH:12][cH:11][c:10]([N:2]([CH3:1])[C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[cH:18]1>>[CH3:1][N:2]([C:3](=[O:4])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9])[c:10]1[cH:11][cH:12][cH:13][c:14]([N:15]=[C:16]=[O:17])[cH:18]1
CCOC(=O)Cl.CN(C(=O)OC(C)(C)C)c1cccc(C(=O)O)c1
CN(C(=O)OC(C)(C)C)c1cccc(N=C=O)c1
null
null
C1(=CC=CC=C1)C.O.CC(=O)C
Protection
OtherReaction
c10a61766aae74484ca819d3bc673441d5a3ac212905587e31e25acab95896c9
ad3ce9de5d008e6fe42518a159a24df64edec84808853d24edaa142b8df8c38e
c1ccccc1
C-C-O-[C;H0;D3;+0:1](-Cl)=[O;D1;H0:2].O-C(=O)-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6]:[c:7]>>[O;D1;H0:2]=[C;H0;D2;+0:1]=[#7:8]-[c;H0;D3;+0:3](:[c:4]:[c:5]):[c:6]:[c:7]
78.5
[{"value": 78.0, "product": "O(C(C)(C)C)C(=O)N(C)C=1C=C(C=CC1)N=C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.5, "product": "O(C(C)(C)C)C(=O)N(C)C=1C=C(C=CC1)N=C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Et3N (3.71 g, 36.7 mmol) and a solution of ethyl chloroformate (4.31 g, 39.7 mmol) in acetone (10 ml) were successively added dropwise to a solution of 3-(N-tert-butoxylcarbonyl-N-methylamino)benzoic acid (8.0 g, 31.8 mmol) in acetone (64 ml) below 5° C. After stirring for 30 min, a solution of NaN3 (3.10 g, 47.7 mmol)...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Carboxylic acid.Ether
Isocyanate
c1ccccc1
c1ccccc1
c1ccccc1
HCl
C1(=CC=CC=C1)C.O.CC(=O)C
null
0.5
CCOC(=O)Cl.CN(C(=O)OC(C)(C)C)c1cccc(C(=O)O)c1>C1(=CC=CC=C1)C.O.CC(=O)C>CN(C(=O)OC(C)(C)C)c1cccc(N=C=O)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d183881774224975a1ab61e1760c6bad
Cc1ccc(S(=O)(=O)Cl)cc1.OCC(O)CO>>Cc1ccc(S(=O)(=O)OCC(O)COS(=O)(=O)c2ccc(C)cc2)cc1
C1(=CC=C(C=C1)S(=O)(=O)Cl)C.OCC(O)CO.Cl>>S(=O)(=O)(C1=CC=C(C)C=C1)OCC(O)COS(=O)(=O)C1=CC=C(C)C=C1
Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:26][cH:25]1)(=[O:7])=[O:8].[OH:9][CH2:10][CH:11]([OH:12])[CH2:22][OH:14]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[O:9][CH2:10][CH:11]([OH:12])[CH2:13][O:14][S:15](=[O:16])(=[O:17])[c:18]2[cH:19][cH:20][c:21]([CH3:22])[cH:23][cH:24]2)[cH:25][cH:26]1
Cc1ccc(S(=O)(=O)Cl)cc1.OCC(O)CO
Cc1ccc(S(=O)(=O)OCC(O)COS(=O)(=O)c2ccc(C)cc2)cc1
null
null
N1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
051c238cc697fb95d521a378790a706996235c75768c9bc7f5f19c4bbb363bb0
be3f629adcb32a776ba877fc0c1beb58f88fbbb93daba66fe1621aea210f656a
O=S(=O)(OCCCOS(=O)(=O)c1ccccc1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[O;D1;H1:7]-[CH;D3;+0:8](-[C:9]-[OH;D1;+0:10])-[CH2;D2;+0:11]-[OH;D1;+0:12]>>[CH3;D1;+0:11]-[c:13](:[c:14]):[c:15].[O;D1;H0:16]=[#16:17](=[O;D1;H0:18])(-[c:19])-[O;H0;D2;+0:12]-[C:20]-[CH;D3;+0:8](-[O;D1;H1:7])-[C:9]-[O;H0;D2;+0:10]-[S;H0;D4;+0:1](=[O;D1...
null
[]
null
null
null
null
Compound 2 was synthesized according to the previous reported method with modifications (Benbouzid et al., 1988). p-Toluenesulfonyl chloride (10.29 g, 54 mmol) dissolved in dry pyridine was added to a stirred solution of anhydrous glycerol (2.48 g, 27 mmol) in dry pyridine (30 ml at 0° C.). The solution was added slowl...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Primary alcohol.Primary alcohol.Secondary alcohol.Sulfonyl halide
Tosylate.Tosylate.Secondary alcohol
null
c1ccccc1
c1ccccc1.c1ccccc1
null
N1=CC=CC=C1
null
null
Cc1ccc(S(=O)(=O)Cl)cc1.OCC(O)CO>N1=CC=CC=C1>Cc1ccc(S(=O)(=O)OCC(O)COS(=O)(=O)c2ccc(C)cc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0fdf59899d7d46d0ae418ee316a592b9
CCCCc1nc(Cl)c(CO)[nH]1>>CCCCc1nc(Cl)c(C=O)[nH]1
C(CCC)C=1NC(=C(N1)Cl)CO.O>>C(CCC)C=1NC(=C(N1)Cl)C=O
[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([Cl:8])[c:9]([CH2:10][OH:11])[nH:12]1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([Cl:8])[c:9]([CH:10]=[O:11])[nH:12]1
CCCCc1nc(Cl)c(CO)[nH]1
CCCCc1nc(Cl)c(C=O)[nH]1
null
[O-2].[O-2].[Mn+4]
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1c[nH]cn1
[Cl;D1;H0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1-[CH2;D2;+0:7]-[OH;D1;+0:8]>>[Cl;D1;H0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1-[CH;D2;+0:7]=[O;H0;D1;+0:8]
86.3
[{"value": 86.0, "product": "C(CCC)C=1NC(=C(N1)Cl)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.3, "product": "C(CCC)C=1NC(=C(N1)Cl)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A stirred mixture of 2-n-butyl-4-chloro-5-hydroxymethylimidazole (15.00 g, 0.0795 mol) and activated manganese dioxide (40.00 g) in 600 ml of methylene chloride was refluxed for 24 h using a water separator. The mixture was filtered hot through a Celite® pad. The Celite® pad was washed several times with hot methylene ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1c[nH]cn1
null
[O-2].[O-2].[Mn+4].C(Cl)Cl
null
null
CCCCc1nc(Cl)c(CO)[nH]1>[O-2].[O-2].[Mn+4].C(Cl)Cl>CCCCc1nc(Cl)c(C=O)[nH]1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2843bd13368f422ab3826093b175bc25
CCCCC(=N)N.CCO.COC(=O)C=CC=O>>CCCCc1nc(CC(=O)OCC)c[nH]1
C(=O)C=CC(=O)OC.[H-].[Na+].C(C)O.Cl.C(CCCC)(=N)N>>C(CCC)C=1NC=C(N1)CC(=O)OCC
[CH3:1][CH2:2][CH2:3][CH2:4][C:5](=[NH:6])[NH2:15].OC[CH3:13].O=[CH:14][CH:7]=[CH:8][C:9](=[O:10])[O:11][CH3:12]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([CH2:8][C:9](=[O:10])[O:11][CH2:12][CH3:13])[cH:14][nH:15]1
CCCCC(=N)N.CCO.COC(=O)C=CC=O
CCCCc1nc(CC(=O)OCC)c[nH]1
null
null
C1=CC=CC=C1
Aromatic Heterocycle Formation
OtherReaction
f6d52ea8c1ef3a677e8faa4e6193cce69d7709e564ab85a4c0c46d0a6694d531
373cfe5f2ced9afde13ee4279ab98d0c57bacbc28362be854cec0c75098b2267
c1c[nH]cn1
O-C-[CH3;D1;+0:1].O=[CH;D2;+0:2]-[CH;D2;+0:3]=[CH;D2;+0:4]-[C:5](=[O;D1;H0:6])-[#8:7]-[CH3;D1;+0:8].[C:9]-[C:10]-[C;H0;D3;+0:11](-[NH2;D1;+0:12])=[NH;D1;+0:13]>>[C:9]-[C:10]-[c;H0;D3;+0:11]1:[n;H0;D2;+0:13]:[c;H0;D3;+0:3](-[CH2;D2;+0:4]-[C:5](=[O;D1;H0:6])-[#8:7]-[CH2;D2;+0:8]-[CH3;D1;+0:1]):[cH;D2;+0:2]:[nH;D2;+0:12]:...
null
[]
null
null
null
null
Sodium hydride (2.82 g, 0,117 mol) was dissolved in 30 ml of absolute ethanol at 0° C. Valeramidine hydrochloride (16.71 g, 0.123 mol) was added to this solution, and after 15 minutes the solution was filtered and the collected solid was washed with 20 ml of ethanol and 50 ml of benzene. The combined filtrates were dil...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester.Primary alcohol.Primary amine
Ester
null
c1c[nH]cn1
c1c[nH]cn1
HO-
C1=CC=CC=C1
null
null
CCCCC(=N)N.CCO.COC(=O)C=CC=O>C1=CC=CC=C1>CCCCc1nc(CC(=O)OCC)c[nH]1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-132a212c419b44f6b52e3b5ef79af5b4
CCCCc1nc(CO)c[nH]1.O=C1CCC(=O)N1I>>CCCCc1nc(I)c(CO)[nH]1
IN1C(CCC1=O)=O.C(CCC)C=1NC=C(N1)CO>>C(CCC)C=1NC(=C(N1)I)CO
[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[nH:6][cH:7][c:9]([CH2:10][OH:11])[n:12]1.O=C1CCC(=O)N1[I:8]>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([I:8])[c:9]([CH2:10][OH:11])[nH:12]1
CCCCc1nc(CO)c[nH]1.O=C1CCC(=O)N1I
CCCCc1nc(I)c(CO)[nH]1
null
null
C(C)O.O
Functional Group Interconversion
OtherReaction
339179e6c50945dd3ac07a96a57059a7154e475073d7636ad2fc68e36469c54f
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1c[nH]cn1
O=C1-C-C-C(=O)-N-1-[I;H0;D1;+0:1].[C:2]-[c:3]1:[cH;D2;+0:4]:[nH;D2;+0:5]:[c:6](-[C:7]):[n;H0;D2;+0:8]:1>>[C:2]-[c:3]1:[nH;D2;+0:8]:[c:6](-[C:7]):[n;H0;D2;+0:5]:[c;H0;D3;+0:4]:1-[I;H0;D1;+0:1]
95
[{"value": 95.0, "product": "C(CCC)C=1NC(=C(N1)I)CO", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
N-iodosuccinimide (148.75 g, 0.661 mol) was added to a stirred solution of 2-n-butyl-4-hydroxymethylimidazole (100.78 g, 0.652 mol) in 500 ml of absolute ethanol. After 20 minutes the solution was heated to 40°-45° C. for 45 minutes, diluted with 2.5 L of water, and chilled. The crystalline product which formed was col...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1c[nH]cn1.C1CCNC1
c1c[nH]cn1
c1c[nH]cn1
HO-
C(C)O.O
null
null
CCCCc1nc(CO)c[nH]1.O=C1CCC(=O)N1I>C(C)O.O>CCCCc1nc(I)c(CO)[nH]1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-de21b1de13124c589802a272f7412025
CCCCc1nc(I)c(CO)[nH]1>>CCCCc1nc(I)c(C=O)[nH]1
C(CCC)C=1NC(=C(N1)I)CO>>C(CCC)C=1NC(=C(N1)I)C=O
[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([I:8])[c:9]([CH2:10][OH:11])[nH:12]1>>[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([I:8])[c:9]([CH:10]=[O:11])[nH:12]1
CCCCc1nc(I)c(CO)[nH]1
CCCCc1nc(I)c(C=O)[nH]1
null
[O-2].[O-2].[Mn+4]
ClCCl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1c[nH]cn1
[I;D1;H0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1-[CH2;D2;+0:7]-[OH;D1;+0:8]>>[I;D1;H0:1]-[c:2]1:[#7;a:3]:[c:4]:[#7;a:5]:[c:6]:1-[CH;D2;+0:7]=[O;H0;D1;+0:8]
84.2
[{"value": 84.0, "product": "C(CCC)C=1NC(=C(N1)I)C=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.2, "product": "C(CCC)C=1NC(=C(N1)I)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A stirred mixture of 174.1 g (0.62 mol) of 2-n-butyl-5-hydroxymethyl-4-iodoimidazole and 360 g (4.14 mol) of manganese dioxide in 3 L of dichloromethane was refluxed for 24 hr using a trap to remove water. The hot reaction mixture was filtered through a Celite® pad which was then washed with 4.5 L of boiling methylene ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1c[nH]cn1
null
[O-2].[O-2].[Mn+4].ClCCl
null
null
CCCCc1nc(I)c(CO)[nH]1>[O-2].[O-2].[Mn+4].ClCCl>CCCCc1nc(I)c(C=O)[nH]1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ff9fddba17f84a17b2c77c4ed15d72d3
CCCCc1nc(I)c(C=O)[nH]1.COC(=O)c1ccc(CBr)c2ccccc12>>CCCCC1N=C(I)C(C=O)(Cc2ccc(C(=O)OC)c3ccccc23)N1
C([O-])([O-])=O.[K+].[K+].C(CCC)C=1NC(=C(N1)I)C=O.BrCC1=CC=C(C2=CC=CC=C12)C(=O)OC.O>>C(CCC)C1NC(C(=N1)I)(C=O)CC1=CC=C(C2=CC=CC=C12)C(=O)OC
[CH3:1][CH2:2][CH2:3][CH2:4][c:5]1[n:6][c:7]([I:8])[c:9]([CH:10]=[O:11])[nH:27]1.Br[CH2:12][c:13]1[cH:14][cH:15][c:16]([C:17](=[O:18])[O:19][CH3:20])[c:21]2[cH:22][cH:23][cH:24][cH:25][c:26]12>>[CH3:1][CH2:2][CH2:3][CH2:4][CH:5]1[N:6]=[C:7]([I:8])[C:9]([CH:10]=[O:11])([CH2:12][c:13]2[cH:14][cH:15][c:16]([C:17](=[O:18])...
CCCCc1nc(I)c(C=O)[nH]1.COC(=O)c1ccc(CBr)c2ccccc12
CCCCC1N=C(I)C(C=O)(Cc2ccc(C(=O)OC)c3ccccc23)N1
null
null
CN(C=O)C
C-C Coupling
OtherReaction
d8c74bd68b3292fafed319bd6ec34baf915d17a5e15132d7b20991dcb6ff2b9a
1fb0e31b83cdc0f1a3d139358556d22838f4ec7845f0c3ac45c5d2b6cea2942b
C1=NCNC1Cc1cccc2ccccc12
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[c;H0;D3;+0:7]1:[n;H0;D2;+0:8]:[c;H0;D3;+0:9](-[I;D1;H0:10]):[c;H0;D3;+0:11](-[C:12]=[O;D1;H0:13]):[nH;D2;+0:14]:1>>[C:5]-[C:6]-[CH;D3;+0:7]1-[N;H0;D2;+0:8]=[C;H0;D3;+0:9](-[I;D1;H0:10])-[C;H0;D4;+0:11](-[C:12]=[O;D1;H0:13])(-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[NH;D2;+0:...
85
[{"value": 85.0, "product": "C(CCC)C1NC(C(=N1)I)(C=O)CC1=CC=C(C2=CC=CC=C12)C(=O)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 84.8, "product": "C(CCC)C1NC(C(=N1)I)(C=O)CC1=CC=C(C2=CC=CC=C12)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
15
HOUR
A suspension of 29.53 g (0.214 mol) of powdered potassium carbonate, 60.00 g (0.214 mol) of 2-butyl-4-iodoimidazole-5-carboxaldehyde, and 65.68 g (0.235 mol) of methyl 4-bromomethylnaphthalene-1-carboxylate (E. A. Dixon, A. Fischer, and F. P. Robinson, Can. J. Chem. 59, 2629 (1981)) in 600 ml of dimethylformamide was s...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary halide.Aldehyde
Alkenyl halide.Aldehyde.Secondary amine
c1c[nH]cn1
C1=NCNC1
C1=NCNC1.c1ccc2ccccc2c1
Br-
CN(C=O)C
70
15
CCCCc1nc(I)c(C=O)[nH]1.COC(=O)c1ccc(CBr)c2ccccc12>CN(C=O)C>CCCCC1N=C(I)C(C=O)(Cc2ccc(C(=O)OC)c3ccccc23)N1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f310c91312a24ed185ed64c535694b9b
COc1ccc(C(CC(=O)O)N2C(=O)c3ccccc3C2=O)cc1OC1CCCC1.[NH4+]>>COc1ccc(C(CC(N)=O)N2C(=O)c3ccccc3C2=O)cc1OC1CCCC1
C1(C=2C(C(N1C(CC(=O)O)C1=CC(=C(C=C1)OC)OC1CCCC1)=O)=CC=CC2)=O.C(=O)(N1C=NC=C1)N1C=NC=C1.[OH-].[NH4+]>>C1(C=2C(C(N1C(CC(=O)N)C1=CC(=C(C=C1)OC)OC1CCCC1)=O)=CC=CC2)=O
O[C:9]([CH2:8][CH:7]([c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[c:24]([O:25][CH:26]2[CH2:27][CH2:28][CH2:29][CH2:30]2)[cH:23]1)[N:12]1[C:13](=[O:14])[c:15]2[cH:16][cH:17][cH:18][cH:19][c:20]2[C:21]1=[O:22])=[O:11].[NH4+:10]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH:7]([CH2:8][C:9]([NH2:10])=[O:11])[N:12]2[C:13](=[O:14])[c:15...
COc1ccc(C(CC(=O)O)N2C(=O)c3ccccc3C2=O)cc1OC1CCCC1.[NH4+]
COc1ccc(C(CC(N)=O)N2C(=O)c3ccccc3C2=O)cc1OC1CCCC1
null
CN(C1=CC=NC=C1)C
O1CCCC1
Acylation
Carboxylic acid to amide conversion
1283aef55d7ee699f097a8e5267689198c76ba671644401547f902657820236d
cb0a71c3fb37a76e96fbd81aae6f95a28398a03d1ad2c8e877085e735efb98f1
O=C1c2ccccc2C(=O)N1Cc1cccc(OC2CCCC2)c1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[NH4+;D0:5]>>[C:4]-[C:3]-[C;H0;D3;+0:1](-[NH2;D1;+0:5])=[O;D1;H0:2]
62.2
[{"value": 62.2, "product": "C1(C=2C(C(N1C(CC(=O)N)C1=CC(=C(C=C1)OC)OC1CCCC1)=O)=CC=CC2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
25
CELSIUS
1.5
HOUR
A mixture of 3-phthalimido-3-(3-cyclopentyloxy-4-methoxyphenyl)propionic acid (2.05 g, 5.00 mmol), 1,1'-carbonyldiimidazole (0.91 g, 5.5 mmol) and 4-dimethylaminopyridine (trace) in tetrahydrofuran (20 mL) was stirred for 1.5 hours under nitrogen at approximately 25° C. To the solution was added ammonium hydroxide (1.0...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary amide
null
null
c1ccccc1.c1ccc2c(c1)C[NH]C2.C1CCCC1
HO-
CN(C1=CC=NC=C1)C.O1CCCC1
25
1.5
COc1ccc(C(CC(=O)O)N2C(=O)c3ccccc3C2=O)cc1OC1CCCC1.[NH4+]>CN(C1=CC=NC=C1)C.O1CCCC1>COc1ccc(C(CC(N)=O)N2C(=O)c3ccccc3C2=O)cc1OC1CCCC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-48bcadbbba7b4f4299bd816594d61a87
COc1ccc(C=O)cc1OC1CCCC1.C[Si](C)(C)N[Si](C)(C)C>>CCC(N)c1ccc(OC)c(OC2CCCC2)c1
C(C)[Mg]Br.C(CCC)[Li].C[Si](N[Si](C)(C)C)(C)C.C1(CCCC1)OC=1C=C(C=O)C=CC1OC.[Cl-].[NH4+]>>C1(CCCC1)OC=1C=C(C=CC1OC)C(CC)N
O=[CH:3][c:5]1[cH:6][cH:7][c:8]([O:9][CH3:10])[c:11]([O:12][CH:13]2[CH2:14][CH2:15][CH2:16][CH2:17]2)[cH:18]1.C[Si](C)(C)[NH:4][Si](C)(C)C>>[CH3:1][CH2:2][CH:3]([NH2:4])[c:5]1[cH:6][cH:7][c:8]([O:9][CH3:10])[c:11]([O:12][CH:13]2[CH2:14][CH2:15][CH2:16][CH2:17]2)[cH:18]1
COc1ccc(C=O)cc1OC1CCCC1.C[Si](C)(C)N[Si](C)(C)C
CCC(N)c1ccc(OC)c(OC2CCCC2)c1
null
null
CC#N.CCCCCC.O1CCCC1
Heteroatom Alkylation and Arylation
OtherReaction
13e3e72401395cfde3aa1eedd418837033025f6f253a59da5c4d1e1750b92879
49265bb2bfa9eef218bd07821ad7c78053d001bea6481ce70742cda21ee85079
c1ccc(OC2CCCC2)cc1
C-[Si](-C)(-C)-[NH;D2;+0:1]-[Si](-C)(-C)-C.O=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[C;D1;H3:6]-[C:7]-[CH;D3;+0:2](-[NH2;D1;+0:1])-[c:3](:[c:4]):[c:5]
null
[]
null
null
30
MINUTE
To an ice bath cooled stirred solution of 1,1,1,3,3,3-hexamethyldisilazane (2.5M, 4.1 mL, 19.5 mmol) in tetrahydrofuran (5 mL) under nitrogen, was added a hexane solution of butyl lithium (7.2 mL, 18 mmol) via syringe. The ice bath was removed and the solution was stirred for 30 minutes at room temperature. This soluti...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine.Silyl protective group.Silyl protective group
Primary amine
null
null
c1ccccc1.C1CCCC1
HO-
CC#N.CCCCCC.O1CCCC1
null
0.5
COc1ccc(C=O)cc1OC1CCCC1.C[Si](C)(C)N[Si](C)(C)C>CC#N.CCCCCC.O1CCCC1>CCC(N)c1ccc(OC)c(OC2CCCC2)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a172f4e4b1614e5bac954c6d01d97ff6
COc1ccc(C=O)cc1OC1CCc2ccccc21.C[Si](C)(C)N[Si](C)(C)C>>CCC(N)c1ccc(OC)c(OC2CCc3ccccc32)c1
C(C)[Mg]Br.C(CCC)[Li].C[Si](N[Si](C)(C)C)(C)C.C1(CCC2=CC=CC=C12)OC=1C=C(C=O)C=CC1OC.[Cl-].[NH4+]>>C1(CCC2=CC=CC=C12)OC=1C=C(C=CC1OC)C(CC)N
O=[CH:3][c:5]1[cH:6][cH:7][c:8]([O:9][CH3:10])[c:11]([O:12][CH:13]2[CH2:14][CH2:15][c:16]3[cH:17][cH:18][cH:19][cH:20][c:21]32)[cH:22]1.C[Si](C)(C)[NH:4][Si](C)(C)C>>[CH3:1][CH2:2][CH:3]([NH2:4])[c:5]1[cH:6][cH:7][c:8]([O:9][CH3:10])[c:11]([O:12][CH:13]2[CH2:14][CH2:15][c:16]3[cH:17][cH:18][cH:19][cH:20][c:21]32)[cH:22...
COc1ccc(C=O)cc1OC1CCc2ccccc21.C[Si](C)(C)N[Si](C)(C)C
CCC(N)c1ccc(OC)c(OC2CCc3ccccc32)c1
null
null
CC#N.CCCCCC.O1CCCC1
Heteroatom Alkylation and Arylation
OtherReaction
13e3e72401395cfde3aa1eedd418837033025f6f253a59da5c4d1e1750b92879
49265bb2bfa9eef218bd07821ad7c78053d001bea6481ce70742cda21ee85079
c1ccc(OC2CCc3ccccc32)cc1
C-[Si](-C)(-C)-[NH;D2;+0:1]-[Si](-C)(-C)-C.O=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[C;D1;H3:6]-[C:7]-[CH;D3;+0:2](-[NH2;D1;+0:1])-[c:3](:[c:4]):[c:5]
9
[{"value": 9.0, "product": "C1(CCC2=CC=CC=C12)OC=1C=C(C=CC1OC)C(CC)N", "details": "PERCENTYIELD", "is_desired": false}]
null
null
25
MINUTE
To an ice bath cooled stirred solution of 1,1,1,3,3,3-hexamethyldisilazane (2.7 mL, 13 mmol) in tetrahydrofuran (5 mL) under nitrogen, was added a hexane solution of butyl lithium (2.5M, 4.8 mL, 12 mmol) via syringe. The ice bath was removed and the solution was stirred for 25 minutes at room temperature. This solution...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine.Silyl protective group.Silyl protective group
Primary amine
null
null
c1ccccc1.c1ccc2c(c1)CCC2
HO-
CC#N.CCCCCC.O1CCCC1
null
0.416667
COc1ccc(C=O)cc1OC1CCc2ccccc21.C[Si](C)(C)N[Si](C)(C)C>CC#N.CCCCCC.O1CCCC1>CCC(N)c1ccc(OC)c(OC2CCc3ccccc32)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e365fd6c4897470482774680a6343b87
CCOc1ccc(C(CC(N)=O)N2C(=O)c3ccccc3C2=O)cc1OCC>>CCOc1ccc(C(CC#N)N2C(=O)c3ccccc3C2=O)cc1OCC
CC#N.OP(=O)(O)O.C(=O)(O)[O-].[Na+].C1(C=2C(C(N1C(CC(=O)N)C1=CC(=C(C=C1)OCC)OCC)=O)=CC=CC2)=O.CN1CCOCC1.S(=O)(Cl)Cl>>C1(C=2C(C(N1C(CC#N)C1=CC(=C(C=C1)OCC)OCC)=O)=CC=CC2)=O
O=[C:10]([CH2:9][CH:8]([c:7]1[cH:6][cH:5][c:4]([O:3][CH2:2][CH3:1])[c:24]([O:25][CH2:26][CH3:27])[cH:23]1)[N:12]1[C:13](=[O:14])[c:15]2[cH:16][cH:17][cH:18][cH:19][c:20]2[C:21]1=[O:22])[NH2:11]>>[CH3:1][CH2:2][O:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH2:9][C:10]#[N:11])[N:12]2[C:13](=[O:14])[c:15]3[cH:16][cH:17][cH:18][cH:...
CCOc1ccc(C(CC(N)=O)N2C(=O)c3ccccc3C2=O)cc1OCC
CCOc1ccc(C(CC#N)N2C(=O)c3ccccc3C2=O)cc1OCC
null
null
CN(C)C=O
Miscellaneous
OtherReaction
5094e9d814705bbdc421edbf7e9198e499e70e93916e2cec6eefbc82d1ba5440
32b9893bcb5223559a9d02852f8392cf6473aacfb044a52ba4e9cb9c29edb170
O=C1c2ccccc2C(=O)N1Cc1ccccc1
O=[C;H0;D3;+0:1](-[NH2;D1;+0:2])-[C:3]-[C:4]>>[C:4]-[C:3]-[C;H0;D2;+0:1]#[N;H0;D1;+0:2]
55
[{"value": 55.0, "product": "C1(C=2C(C(N1C(CC#N)C1=CC(=C(C=C1)OCC)OCC)=O)=CC=CC2)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 54.9, "product": "C1(C=2C(C(N1C(CC#N)C1=CC(=C(C=C1)OCC)OCC)=O)=CC=CC2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To an ice bath cooled stirred suspension of 3-phthalimido-3-(3,4-diethoxyphenyl)propionamide (0.96 g, 2.5 mmol) and 4-methylmorpholine (0.66 mL, 6 mmol) in DMF (9 mL) under nitrogen, was added thionyl chloride (0.35 mL, 4.8 mmol) dropwise. There was a slight exotherm after which the mixture was stirred at 0°-5° C. for ...
10.6084/m9.figshare.5104873.v1
null
Primary amide
Nitrile
null
null
c1ccccc1.c1ccc2c(c1)C[NH]C2
HO-
CN(C)C=O
null
null
CCOc1ccc(C(CC(N)=O)N2C(=O)c3ccccc3C2=O)cc1OCC>CN(C)C=O>CCOc1ccc(C(CC#N)N2C(=O)c3ccccc3C2=O)cc1OCC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2751c75ddf0c486a8d95a650128f9c7e
C/C=C\C.O.O=C1CCCCC1>>C1=CCOC2(CCCCC2)OC1
C\C=C/C.C1(CCCCC1)=O.O>>C1CCCCC12OCC=CCO2
[CH:1](=[CH:2]\[CH3:3])\[CH3:12].[OH2:11].[O:4]=[C:5]1[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]1>>[CH:1]1=[CH:2][CH2:3][O:4][C:5]2([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10]2)[O:11][CH2:12]1
C/C=C\C.O.O=C1CCCCC1
C1=CCOC2(CCCCC2)OC1
null
null
C1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
a8e59b804e0a5a5ee2234051e1e76f1119fd05c6f713dec2babad68cb085ae6d
6c57eaf115312957a9a907ba5f895cbf506b497e86f310f03cc08f79ec3ac645
C1=CCOC2(CCCCC2)OC1
[CH3;D1;+0:1]/[C:2]=[C:3]\[CH3;D1;+0:4].[C:5]-[C:6]-[C;H0;D3;+0:7](=[O;H0;D1;+0:8])-[C:9]-[C:10].[OH2;D0;+0:11]>>[C:5]-[C:6]-[C;H0;D4;+0:7]1(-[C:9]-[C:10])-[O;H0;D2;+0:11]-[CH2;D2;+0:1]-[C:2]=[C:3]-[CH2;D2;+0:4]-[O;H0;D2;+0:8]-1
92
[{"value": 92.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Cis-but-2-ene, 4-diol (50 g), cyclohexanone (50 g) and SNCA catalyst (2.5 g) were refluxed in benzene (75 ml) using a Deanstark water separator. The catalyst was filtered, the solvent evaporated and the residue distilled at 80°-85° C./4 torr to give 7,12-dioxaspiro[5,6]dodec-9-ene of formula III (92%) of the drawings. ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Ether.Ether
C1CCCCC1
C1=CCOC2(CCCCC2)OC1
C1=CCOC2(CCCCC2)OC1
null
C1=CC=CC=C1
null
null
C/C=C\C.O.O=C1CCCCC1>C1=CC=CC=C1>C1=CCOC2(CCCCC2)OC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-68ed201820eb41f482bf2de3bfa7daba
O=CC1CCOC2(CCCCC2)OC1>>OCC1CCOC2(CCCCC2)OC1
C(=O)C1COC2(CCCCC2)OCC1.[BH4-].[Na+]>>OCC1COC2(CCCCC2)OCC1
[O:1]=[CH:2][CH:3]1[CH2:4][CH2:5][O:6][C:7]2([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)[O:13][CH2:14]1>>[OH:1][CH2:2][CH:3]1[CH2:4][CH2:5][O:6][C:7]2([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)[O:13][CH2:14]1
O=CC1CCOC2(CCCCC2)OC1
OCC1CCOC2(CCCCC2)OC1
null
null
CO
Reduction
Reduction of aldehydes and ketones to alcohols
e7895795cd3f75445716c94697823c5929dcd4b5344525875fe75d36bca2f9d7
21bb81d5469aaaca71ab12c186bea4016451717fad8780cf288858a7d8fbc55a
C1CCC2(CC1)OCCCCO2
[#8:1]-[C:2]-[C:3](-[CH;D2;+0:4]=[O;H0;D1;+0:5])-[C:6]>>[#8:1]-[C:2]-[C:3](-[CH2;D2;+0:4]-[OH;D1;+0:5])-[C:6]
null
[]
10
CELSIUS
null
null
To a solution of 9-formyl-7, 12-dioxaspiro[5,6]dodecane of formula IV (5 g) in methanol (15 ml) was added in small portions NaBH4 (0.5 g) while stirring the solution and maintaining the temperature at 10° C. After complete addition, the reaction mixture was stirred for 3 hr at 20° C. The product residue obtained after ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Primary alcohol
null
null
C1CCC2(CC1)OCCCCO2
null
CO
10
null
O=CC1CCOC2(CCCCC2)OC1>CO>OCC1CCOC2(CCCCC2)OC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-41c36e816c8a49348cb7de1b22c2c650
OCC1CCOC2(CCCCC2)OC1>>OCCC1COC2(CCCCC2)OC1
O.OCC1COC2(CCCCC2)OCC1.C1(=CC=C(C=C1)S(=O)(=O)O)C>>OCCC1COC2(CCCCC2)OC1
[OH:1][CH2:2][CH:3]1[CH2:4][CH2:5][O:6][C:7]2([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)[O:13][CH2:14]1>>[OH:1][CH2:2][CH2:3][CH:4]1[CH2:5][O:6][C:7]2([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)[O:13][CH2:14]1
OCC1CCOC2(CCCCC2)OC1
OCCC1COC2(CCCCC2)OC1
null
null
C1=CC=CC=C1
Miscellaneous
OtherReaction
ab9c52a3476cf18303bd43755898a9308c36629ed14c627b72ab190f6929f44e
bced64702950df7cf56df22d8c2487b007734fece951727fd2c8a1c63fbcf6cc
C1CCC2(CC1)OCCCO2
[O;D1;H1:1]-[C:2]-[CH;D3;+0:3]1-[CH2;D2;+0:4]-[#8:5]-[C:6]-[#8:7]-[C:8]-[CH2;D2;+0:9]-1>>[O;D1;H1:1]-[C:2]-[CH2;D2;+0:3]-[CH;D3;+0:9]1-[C:8]-[#8:7]-[C:6]-[#8:5]-[CH2;D2;+0:4]-1
70
[{"value": 70.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of 9-hydroxymethyl-7, 12-dioxaspiro[5,6]dodecane of the formula V (4 g) of the drawings in benzene (15 ml) was stirred at 10° C. for 5 hr with anhydrous p-toluenesulphonic acid (0.2 g). The reaction mixture was made alkaline by adding TEA and water. The benzene layer was separated and the aqueous layer extra...
10.6084/m9.figshare.5104873.v1
null
Ether
Ether
C1CCC2(CC1)OCCCCO2
C1CCC2(CC1)OCCCO2
C1CCC2(CC1)OCCCO2
null
C1=CC=CC=C1
null
null
OCC1CCOC2(CCCCC2)OC1>C1=CC=CC=C1>OCCC1COC2(CCCCC2)OC1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f10081548cf4415e81c4b90bffd29a7a
C=CC(C)(C)O.CC[SiH](CC)CC>>CC[Si](CC)(CC)CCC(C)(C)O
CC(C=C)(C)O.C(C)[SiH](CC)CC>>CC(CC[Si](CC)(CC)CC)(C)O
[CH2:8]=[CH:9][C:10]([CH3:11])([CH3:12])[OH:13].[CH3:1][CH2:2][SiH:3]([CH2:4][CH3:5])[CH2:6][CH3:7]>>[CH3:1][CH2:2][Si:3]([CH2:4][CH3:5])([CH2:6][CH3:7])[CH2:8][CH2:9][C:10]([CH3:11])([CH3:12])[OH:13]
C=CC(C)(C)O.CC[SiH](CC)CC
CC[Si](CC)(CC)CCC(C)(C)O
null
[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.C(CCC)O.[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl
C(CCC)O
Miscellaneous
OtherReaction
6cc3f1eadda1112665613ad4e645127424bc2dc3fb86a0dd60a3ed530956e2e3
7be997182052ef72a2b91e5073ef9f506315a8ba0f0d67d5adf9938c2c0d61f5
null
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[O;D1;H1:4])-[CH;D2;+0:5]=[CH2;D1;+0:6].[C;D1;H3:7]-[C:8]-[SiH;D3;+0:9](-[C:10]-[C;D1;H3:11])-[C:12]-[C;D1;H3:13]>>[C;D1;H3:1]-[C:2](-[C;D1;H3:3])(-[O;D1;H1:4])-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[Si;H0;D4;+0:9](-[C:8]-[C;D1;H3:7])(-[C:10]-[C;D1;H3:11])-[C:12]-[C;D1;H3:13]
81.1
[{"value": 81.1, "product": "CC(CC[Si](CC)(CC)CC)(C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
null
null
Into a four-necked 500 mL-flask equipped with a stirring apparatus, a thermometer and a dropping funnel, 81.2 g (0.943 mole) of 3-methyl-1-buten-3-ol and 0.2 g of an n-butanol solution containing chloroplatinic acid at a concentration of 2 weight % were charged, and they were heated to 80° C. with stirring. From the dr...
10.6084/m9.figshare.5104873.v1
null
Vinyl
Silyl protective group
null
null
null
null
[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.C(CCC)O.[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.C(CCC)O
80
null
C=CC(C)(C)O.CC[SiH](CC)CC>[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.C(CCC)O.[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl.C(CCC)O>CC[Si](CC)(CC)CCC(C)(C)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-623e76f5d131438c908eae7b5ce8e7ac
C=CC(=O)O.COc1ccc(Br)cc1>>COc1ccc(C=CC(=O)O)cc1
BrC1=CC=C(C=C1)OC.C(C=C)(=O)O.C(C)N(CC)CC>>COC1=CC=C(C=CC(=O)O)C=C1
[CH2:7]=[CH:8][C:9](=[O:10])[OH:11].Br[c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:13][cH:12]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH:7]=[CH:8][C:9](=[O:10])[OH:11])[cH:12][cH:13]1
C=CC(=O)O.COc1ccc(Br)cc1
COc1ccc(C=CC(=O)O)cc1
null
Cl[Pd]Cl
O
C-C Coupling
Heck terminal vinyl
55becfded1a3842d5a03bbf3e1610411c659aff0806930400c4db2ef61f9c87f
4b186811a4930853b446d93d9faa39b267bddb9ce0b8021bda5c5a3b2bc69f0b
c1ccccc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[CH2;D1;+0:6]=[C:7]-[C:8](=[O;D1;H0:9])-[O;D1;H1:10]>>[O;D1;H0:9]=[C:8](-[O;D1;H1:10])-[C:7]=[CH;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
81.2
[{"value": 81.2, "product": "COC1=CC=C(C=CC(=O)O)C=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
130
CELSIUS
null
null
p-bromo anisole (8.4 g), acrylic acid (3.9 g), water (13.5 g), PdCl2 (0.3 mg) and triethyamine (14.3 g, 89.3% pure by titration, the balance being water, recovered by phase separation from a previous run) were charged into an autoclave and heated for 2 hours at 130° C. The work up detailed in Example 1 gave 6.5 g (81%)...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Vinyl
null
c1ccccc1
c1ccccc1
c1ccccc1
HBr
Cl[Pd]Cl.O
130
null
C=CC(=O)O.COc1ccc(Br)cc1>Cl[Pd]Cl.O>COc1ccc(C=CC(=O)O)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-83277f5bcbe3453880c179fb06727b5a
CC(=O)OC(C)=O.O=C(O)c1ccc(O)cc1F>>CC(=O)Oc1ccc(C(=O)O)c(F)c1
FC1=C(C(=O)O)C=CC(=C1)O.C(C)(=O)OC(C)=O>>C(C)(=O)OC1=CC(=C(C(=O)O)C=C1)F
CC(=O)O[C:2]([CH3:1])=[O:3].[OH:4][c:5]1[cH:6][cH:7][c:8]([C:9](=[O:10])[OH:11])[c:12]([F:13])[cH:14]1>>[CH3:1][C:2](=[O:3])[O:4][c:5]1[cH:6][cH:7][c:8]([C:9](=[O:10])[OH:11])[c:12]([F:13])[cH:14]1
CC(=O)OC(C)=O.O=C(O)c1ccc(O)cc1F
CC(=O)Oc1ccc(C(=O)O)c(F)c1
null
S(O)(O)(=O)=O
O
Acylation
Acetic anhydride and alcohol to ester
55f321cc520ab80a97c517ea4db1ffe6ba0ea312e2db70f74b0966421bec0a44
96218bff9f96200922f4dff3481116557fe6986cba41ef7bff8cc8a0b43bd224
c1ccccc1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
80
CELSIUS
null
null
4.3 Grams of 2-fluoro-4-hydroxybenzoic acid and 8.4 g of acetic anhydride were placed in a two-necked flask and mixed. While the mixture was cooled with water, 5 drops of sulfuric acid was added. After the heat generation ended, the mixture was heated at 80° C. for 30 minutes. Then, the reaction mixture was poured into...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Aromatic alcohol
Ester
null
null
c1ccccc1
HO-
S(O)(O)(=O)=O.O
80
null
CC(=O)OC(C)=O.O=C(O)c1ccc(O)cc1F>S(O)(O)(=O)=O.O>CC(=O)Oc1ccc(C(=O)O)c(F)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-2416e9807d124e3c9adcf5213d44dca1
CCCCC[PH](=O)CCCCC.ClP(Cl)Cl>>CCCCCP(Cl)CCCCC
BrCCCCC.C(CCCC)P(CCCCC)=O.P(Cl)(Cl)Cl>>ClP(CCCCC)CCCCC
O=[PH:6]([CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].ClP(Cl)[Cl:7]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][P:6]([Cl:7])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
CCCCC[PH](=O)CCCCC.ClP(Cl)Cl
CCCCCP(Cl)CCCCC
null
null
null
Functional Group Interconversion
OtherReaction
42af6cdfb86a130c92365e01a31b50705eea7bdf12f67dc370bf24402f7ceedc
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
null
Cl-P(-Cl)-[Cl;H0;D1;+0:1].O=[PH;D3;+0:2](-[C:3]-[C:4])-[C:5]-[C:6]>>[C:4]-[C:3]-[P;H0;D3;+0:2](-[Cl;H0;D1;+0:1])-[C:5]-[C:6]
null
[]
null
null
null
null
Following the procedure of Example 3, 1-bromopentane (181.2 g) was used as starting material to prepare di-n-pentylphosphine oxide (22.4 g), and this compound was further reacted with phosphorus trichloride to give chloro di-n-pentylphosphine, b.p. 88° C. at a pressure of 0.3 mm of mercury. This compound (10.4 g) was a...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
HCl
null
null
null
CCCCC[PH](=O)CCCCC.ClP(Cl)Cl>>CCCCCP(Cl)CCCCC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4e1b2e431c034625a9d3cefb9103c42d
CCCC(C)Br.CCCCOP(=O)([O-])OCCCC.CCC[CH](C)[Mg][Br]>>CCCC(C)[PH](=O)C(C)CCC
P(=O)(OCCCC)(OCCCC)[O-].BrC(C)CCC.[Mg].S(O)(O)(=O)=O.CC(CCC)[Mg]Br>>CC(CCC)P(C(C)CCC)=O
Br[CH:4]([CH2:3][CH2:2][CH3:1])[CH3:5].CCCCO[P:6](=O)(OCCCC)[O-:7].[Br][Mg][CH:8]([CH3:9])[CH2:10][CH2:11][CH3:12]>>[CH3:1][CH2:2][CH2:3][CH:4]([CH3:5])[PH:6](=[O:7])[CH:8]([CH3:9])[CH2:10][CH2:11][CH3:12]
CCCC(C)Br.CCCCOP(=O)([O-])OCCCC.CCC[CH](C)[Mg][Br]
CCCC(C)[PH](=O)C(C)CCC
null
null
O1CCCC1.C(C)OCC
Miscellaneous
OtherReaction
bc46d22f8fd7373712bd6257e5bb2db15253d0fdc7b45372c6127c408ee0ba3b
1c6e19e36a4ffeed138891b863c1e8d9668014808d1141eef3237f611a831e96
null
Br-[CH;D3;+0:1](-[C;D1;H3:2])-[C:3]-[C:4].C-C-C-C-O-[P;H0;D4;+0:5](=O)(-[O-;H0;D1:6])-O-C-C-C-C.[Br]-[Mg]-[CH;D3;+0:7](-[C;D1;H3:8])-[C:9]-[C:10]>>[C:10]-[C:9]-[CH;D3;+0:7](-[C;D1;H3:8])-[PH;D3;+0:5](=[O;H0;D1;+0:6])-[CH;D3;+0:1](-[C;D1;H3:2])-[C:3]-[C:4]
52.6
[{"value": 52.6, "product": "CC(CCC)P(C(C)CCC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
10
CELSIUS
1
HOUR
A Grignard solution prepared from 2-bromopentane (227.3 g, 1.5 moles) and magnesium (39.6 g) in tetrahydrofuran (500 cm3) was estimated by a standard procedure and found to contain 1.05 moles of 2-pentyl magnesium bromide. The solution was diluted with diethyl ether (250 cm3) and cooled to 10° C. in an atmosphere of ni...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Secondary halide
null
null
null
null
HBr.Mg
O1CCCC1.C(C)OCC
10
1
CCCC(C)Br.CCCCOP(=O)([O-])OCCCC.CCC[CH](C)[Mg][Br]>O1CCCC1.C(C)OCC>CCCC(C)[PH](=O)C(C)CCC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e7d8772123ce4e13a0605b2c4b96576a
CCC[CH2][Mg][Cl].C[C](C)(C)[Mg][Cl].ClP(Cl)Cl>>CCCCP(Cl)C(C)(C)C
C(C)(C)(C)[Mg]Cl.P(Cl)(Cl)Cl.C(CCC)[Mg]Cl>>C(CCC)P(Cl)C(C)(C)C
[Cl][Mg][CH2:4][CH2:3][CH2:2][CH3:1].[Cl][Mg][C:7]([CH3:8])([CH3:9])[CH3:10].Cl[P:5](Cl)[Cl:6]>>[CH3:1][CH2:2][CH2:3][CH2:4][P:5]([Cl:6])[C:7]([CH3:8])([CH3:9])[CH3:10]
CCC[CH2][Mg][Cl].C[C](C)(C)[Mg][Cl].ClP(Cl)Cl
CCCCP(Cl)C(C)(C)C
null
null
C(C)OCC
Miscellaneous
OtherReaction
448099601124fb8afc117e286cdaae18f0245af2a68c13e2e971c18b863f6b67
5b2a4af98860610907e140d97ebfaf696209e389093bac2abfdbece94c83a55f
null
Cl-[P;H0;D3;+0:1](-Cl)-[Cl;D1;H0:2].[C;D1;H3:3]-[C;H0;D4;+0:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[Mg]-[Cl].[C:7]-[C:8]-[CH2;D2;+0:9]-[Mg]-[Cl]>>[C:7]-[C:8]-[CH2;D2;+0:9]-[P;H0;D3;+0:1](-[Cl;D1;H0:2])-[C;H0;D4;+0:4](-[C;D1;H3:3])(-[C;D1;H3:5])-[C;D1;H3:6]
null
[]
-25
CELSIUS
30
MINUTE
To a solution of phosphorus trichloride (55 g) in dry diethyl ether (200 cm3) stirred and maintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen a 2 molar solution of tert-butyl magnesium chloride in diethyl ether (200 cm3, solution supplied by Aldrich Chemical Co.) was added during 45 min. After a ...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Magnesium halide
null
null
null
null
Mg
C(C)OCC
-25
0.5
CCC[CH2][Mg][Cl].C[C](C)(C)[Mg][Cl].ClP(Cl)Cl>C(C)OCC>CCCCP(Cl)C(C)(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f09ba275a47d468cb9ceb88c522a8f48
CC[CH](C)[Mg][Cl].C[C](C)(C)[Mg][Cl].ClP(Cl)Cl>>CCC(C)P(Cl)C(C)(C)C
C(C)(C)(C)[Mg]Cl.P(Cl)(Cl)Cl.CC(CC)[Mg]Cl>>CC(CC)P(Cl)C(C)(C)C
[Cl][Mg][CH:3]([CH2:2][CH3:1])[CH3:4].[Cl][Mg][C:7]([CH3:8])([CH3:9])[CH3:10].Cl[P:5](Cl)[Cl:6]>>[CH3:1][CH2:2][CH:3]([CH3:4])[P:5]([Cl:6])[C:7]([CH3:8])([CH3:9])[CH3:10]
CC[CH](C)[Mg][Cl].C[C](C)(C)[Mg][Cl].ClP(Cl)Cl
CCC(C)P(Cl)C(C)(C)C
null
null
C(C)OCC
Miscellaneous
OtherReaction
448099601124fb8afc117e286cdaae18f0245af2a68c13e2e971c18b863f6b67
5b2a4af98860610907e140d97ebfaf696209e389093bac2abfdbece94c83a55f
null
Cl-[P;H0;D3;+0:1](-Cl)-[Cl;D1;H0:2].[C;D1;H3:3]-[C;H0;D4;+0:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[Mg]-[Cl].[C;D1;H3:7]-[C:8]-[CH;D3;+0:9](-[C;D1;H3:10])-[Mg]-[Cl]>>[C;D1;H3:3]-[C;H0;D4;+0:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[P;H0;D3;+0:1](-[Cl;D1;H0:2])-[CH;D3;+0:9](-[C;D1;H3:10])-[C:8]-[C;D1;H3:7]
null
[]
-25
CELSIUS
45
MINUTE
To a solution of phosphorus trichloride (55 g) in dry diethyl ether (200 cm3) stirred and maintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen, a 2 molar solution of tert-butyl magnesium chloride in diethyl ether (200 cm3, solution supplied by Aldrich Chemical Co.) was added during 45 min. After a...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Magnesium halide
null
null
null
null
Mg
C(C)OCC
-25
0.75
CC[CH](C)[Mg][Cl].C[C](C)(C)[Mg][Cl].ClP(Cl)Cl>C(C)OCC>CCC(C)P(Cl)C(C)(C)C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-0308ebab0a1b4896a483600b07def253
Cc1ccc(O)c(C)c1.S=P(Cl)(Cl)Cl>>Cc1ccc(OP(=S)(Cl)Oc2ccc(C)cc2C)c(C)c1
P(=S)(Cl)(Cl)Cl.CC1=C(C=CC(=C1)C)O>>P(=S)(OC1=C(C=C(C=C1)C)C)(OC1=C(C=C(C=C1)C)C)Cl
[CH3:1][c:2]1[cH:3][cH:4][c:5]([OH:6])[c:19]([CH3:20])[cH:21]1.Cl[P:7](Cl)(=[S:8])[Cl:9]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([O:6][P:7](=[S:8])([Cl:9])[O:10][c:11]2[cH:12][cH:13][c:14]([CH3:15])[cH:16][c:17]2[CH3:18])[c:19]([CH3:20])[cH:21]1
Cc1ccc(O)c(C)c1.S=P(Cl)(Cl)Cl
Cc1ccc(OP(=S)(Cl)Oc2ccc(C)cc2C)c(C)c1
null
null
C(C)N(CC)CC
Aromatic Heterocycle Formation
OtherReaction
bf12adbba621223d3feca21c5b95fc7ec55684e22bc36f75ac8bba03ce37ea71
212bb5eaccca98121639811e71e750c4cbfba99e07094c3a0cf2d1400ec85f5f
S=[PH](Oc1ccccc1)Oc1ccccc1
Cl-[P;H0;D4;+0:1](-Cl)(-[Cl;D1;H0:2])=[S;D1;H0:3].[OH;D1;+0:4]-[c:5](:[c:6]):[c:7]>>[Cl;D1;H0:2]-[P;H0;D4;+0:1](=[S;D1;H0:3])(-[#8:8]-[c:9])-[O;H0;D2;+0:4]-[c:5](:[c:6]):[c:7]
89.9
[{"value": 89.9, "product": "P(=S)(OC1=C(C=C(C=C1)C)C)(OC1=C(C=C(C=C1)C)C)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
20
CELSIUS
null
null
Thiophosphoryl chloride (17.0 g) was dissolved in tuoluene (250 cm3) and triethylamine (21.5 g) was added. The solution was stirred at 20° C. and 2,4-dimethylphenol (24.4 g) was added in portions during 1 hr. The mixture was stirred for 2 hr. and then heated and stirred at 80° C. for a further 2 hr. and then cooled and...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
null
null
c1ccccc1
c1ccccc1.c1ccccc1
null
C(C)N(CC)CC
20
null
Cc1ccc(O)c(C)c1.S=P(Cl)(Cl)Cl>C(C)N(CC)CC>Cc1ccc(OP(=S)(Cl)Oc2ccc(C)cc2C)c(C)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-edafaca1912e4767aa73ecb661b50df1
C1CCOC1.CCOP(=S)(Cl)OCC.N.O=S(=O)(O)O>>CCOP(=O)(NP(=S)(OCC)OCC)OCC
P(=S)(OCC)(OCC)Cl.N.O1CCCC1.S(O)(O)(=O)=O>>O(P(OCC)(=S)NP(=O)(OCC)OCC)CC
O1[CH2:2][CH2:1][CH2:14][CH2:13]1.Cl[P:4]([O:3][CH2:10][CH3:11])(=[S:8])[O:15][CH2:16][CH3:17].[NH3:6].O=S(=[O:5])([OH:9])[OH:12]>>[CH3:1][CH2:2][O:3][P:4](=[O:5])([NH:6][P:7](=[S:8])([O:9][CH2:10][CH3:11])[O:12][CH2:13][CH3:14])[O:15][CH2:16][CH3:17]
C1CCOC1.CCOP(=S)(Cl)OCC.N.O=S(=O)(O)O
CCOP(=O)(NP(=S)(OCC)OCC)OCC
null
null
ClCCl
Protection
OtherReaction
b1264ad81432c1a30deb65dcc866383e68d87c295b3970c5ce4335c14e69801b
e5a804eb0b1df43ecdb81750f9496bf5176f3accfd96a6411b341e34f9f5447f
null
Cl-[P;H0;D4;+0:1](=[S;H0;D1;+0:2])(-[#8:3]-[C:4])-[O;H0;D2;+0:5]-[CH2;D2;+0:6]-[C;D1;H3:7].O1-[CH2;D2;+0:8]-[CH2;D2;+0:9]-[CH2;D2;+0:10]-[CH2;D2;+0:11]-1.O=S(=[O;H0;D1;+0:12])(-[OH;D1;+0:13])-[OH;D1;+0:14].[NH3;D0;+0:15]>>[C:4]-[#8:3]-[P;H0;D4;+0:1](=[O;H0;D1;+0:12])(-[NH;D2;+0:15]-[#15:16](=[S;H0;D1;+0:2])(-[O;H0;D2;+...
null
[]
65
CELSIUS
2
HOUR
Diethyl chlorothiophosphate (25.04 g, supplied by Aldrich Chemical Company Ltd.) was added dropwise with stirring to a saturated solution of ammonia in tetrahydrofuran (250 cm3). Stirring was continued for two hr. The mixture was filtered to remove precipitated ammonium chloride and then concentrated by distillation of...
10.6084/m9.figshare.5104873.v1
null
Ether
Secondary amine
C1CCOC1
null
null
HCl
ClCCl
65
2
C1CCOC1.CCOP(=S)(Cl)OCC.N.O=S(=O)(O)O>ClCCl>CCOP(=O)(NP(=S)(OCC)OCC)OCC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4cdef75204d84d62a9005173b427b859
CC[CH](C)[Mg][Cl].ClP(Cl)Cl>>CCC(C)P(Cl)C(C)CC
P(Cl)(Cl)Cl.CC(CC)[Mg]Cl>>CC(CC)P(Cl)C(C)CC
[Cl][Mg][CH:3]([CH2:2][CH3:1])[CH3:4].Cl[P:5](Cl)[Cl:6]>>[CH3:1][CH2:2][CH:3]([CH3:4])[P:5]([Cl:6])[CH:7]([CH3:8])[CH2:9][CH3:10]
CC[CH](C)[Mg][Cl].ClP(Cl)Cl
CCC(C)P(Cl)C(C)CC
null
null
C(C)OCC
C-C Coupling
OtherReaction
ed6fb77c42e402438fb059abb66e2fd1d9dd9b973de8deccb8fe05f61ee9052c
8bca8ca721f0288f0875e75b7f264133e86623956746bda21982177c5da407f2
null
Cl-[P;H0;D3;+0:1](-Cl)-[Cl;D1;H0:2].[C;D1;H3:3]-[C:4]-[CH;D3;+0:5](-[C;D1;H3:6])-[Mg]-[Cl]>>[C:7]-[C:8](-[C;D1;H3:9])-[P;H0;D3;+0:1](-[Cl;D1;H0:2])-[CH;D3;+0:5](-[C;D1;H3:6])-[C:4]-[C;D1;H3:3]
null
[]
null
null
null
null
In the manner of Examples 6 and 7, 2-butyl magnesium chloride (800 cm3 of a 2M solution in diethyl ether supplied by Aldrich Chemical Co.) was reacted with phosphorus trichloride (110 g) in diethyl ether (450 cm3) to give di-2-butylchlorophosphine (77.8 g, b.p. 84° C. at a pressure of 15 mm of mercury), and this compou...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide
null
null
null
null
null
C(C)OCC
null
null
CC[CH](C)[Mg][Cl].ClP(Cl)Cl>C(C)OCC>CCC(C)P(Cl)C(C)CC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-94ebb151cdce429fa9a1e76ab6551460
Cc1cc(Cl)ccc1O.NP(N)(N)=S.S=P(Cl)(Cl)Cl.[O-]P([O-])(=S)Cl>>Cc1cc(Cl)ccc1OP(=O)(NP(=S)(Oc1ccc(Cl)cc1C)Oc1ccc(Cl)cc1C)Oc1ccc(Cl)cc1C
ClC1=CC(=C(C=C1)O)C.[H-].[Na+].P(=S)(N)(N)N.N.P(=S)(Cl)(Cl)Cl.[H-].[Na+].P(=S)([O-])([O-])Cl.P(=S)(N)(N)N>>O(P(OC1=C(C=C(C=C1)Cl)C)(=S)NP(=O)(OC1=C(C=C(C=C1)Cl)C)OC1=C(C=C(C=C1)Cl)C)C1=C(C=C(C=C1)Cl)C
[CH3:1][c:2]1[cH:3][c:4]([Cl:5])[cH:6][cH:7][c:8]1[OH:9].N[P:13](N)([NH2:12])=[S:14].S=P(Cl)([Cl:20])[Cl:38].S=[P:10]([O-:11])([O-:15])[Cl:29]>>[CH3:1][c:2]1[cH:3][c:4]([Cl:5])[cH:6][cH:7][c:8]1[O:9][P:10](=[O:11])([NH:12][P:13](=[S:14])([O:15][c:16]1[cH:17][cH:18][c:19]([Cl:20])[cH:21][c:22]1[CH3:23])[O:24][c:25]1[cH:...
Cc1cc(Cl)ccc1O.NP(N)(N)=S.S=P(Cl)(Cl)Cl.[O-]P([O-])(=S)Cl
Cc1cc(Cl)ccc1OP(=O)(NP(=S)(Oc1ccc(Cl)cc1C)Oc1ccc(Cl)cc1C)Oc1ccc(Cl)cc1C
null
null
C1(=CC=CC=C1)C.CCCCCC.CCOCC.O1CCCC1
Aromatic Heterocycle Formation
OtherReaction
fbc357d27ff55096b0900ea3c41337d8d576fb2aada92aa1cf54f0c27217023d
207ba4347e7ae3f1de3e65e474b89eab295dfec83cd096679dca90feff0c43f0
O=P(NP(=S)(Oc1ccccc1)Oc1ccccc1)(Oc1ccccc1)Oc1ccccc1
Cl-P(=S)(-[Cl;H0;D1;+0:1])-[Cl;H0;D1;+0:2].N-[P;H0;D4;+0:3](-N)(-[NH2;D1;+0:4])=[S;D1;H0:5].S=[P;H0;D4;+0:6](-[Cl;H0;D1;+0:7])(-[O-;H0;D1:8])-[O-;H0;D1:9].[OH;D1;+0:10]-[c:11](:[c:12]):[c:13]>>[Cl;H0;D1;+0:7]-[c:14](:[c:15]):[c:16].[Cl;H0;D1;+0:2]-[c:17](:[c:18]):[c:19].[Cl;H0;D1;+0:1]-[c:20]1:[c:21]:[c:22]:[c:23](-[O;...
null
[]
null
null
3
HOUR
4-chloro-2-methylphenol (142.5 g) was dissolved in a mixture of hexane (200 cm3) and toluene (400 cm3) and sodium hydride (30.0 g of 80% suspension in mineral oil) was added. After stirring for 3 hrs, this suspension was added during 2 hr to a stirred solution of thiophosphoryl chloride (84.5 g) in hexane (100 cm3). Th...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol.Primary amine.Primary amine.Primary amine
Aromatic halide.Aromatic halide.Aromatic halide.Secondary amine
null
c1ccccc1.c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
null
C1(=CC=CC=C1)C.CCCCCC.CCOCC.O1CCCC1
null
3
Cc1cc(Cl)ccc1O.NP(N)(N)=S.S=P(Cl)(Cl)Cl.[O-]P([O-])(=S)Cl>C1(=CC=CC=C1)C.CCCCCC.CCOCC.O1CCCC1>Cc1cc(Cl)ccc1OP(=O)(NP(=S)(Oc1ccc(Cl)cc1C)Oc1ccc(Cl)cc1C)Oc1ccc(Cl)cc1C
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-6780bd14b0b34526b70c2eaf4a175924
Cc1ccc(C(C)C)c(O)c1.S=P(Cl)(Cl)Cl>>Cc1ccc(C(C)C)c(OP(=S)(Cl)Oc2cc(C)ccc2C(C)C)c1
C(C)(C)C1=C(C=C(C=C1)C)O.[H-].[Na+].P(=S)(Cl)(Cl)Cl>>P(=S)(OC1=C(C=CC(=C1)C)C(C)C)(OC1=C(C=CC(=C1)C)C(C)C)Cl
[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]([CH3:7])[CH3:18])[c:9]([OH:10])[cH:25]1.Cl[P:11](Cl)(=[S:12])[Cl:13]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]([CH3:7])[CH3:8])[c:9]([O:10][P:11](=[S:12])([Cl:13])[O:14][c:15]2[cH:16][c:17]([CH3:18])[cH:19][cH:20][c:21]2[CH:22]([CH3:23])[CH3:24])[cH:25]1
Cc1ccc(C(C)C)c(O)c1.S=P(Cl)(Cl)Cl
Cc1ccc(C(C)C)c(OP(=S)(Cl)Oc2cc(C)ccc2C(C)C)c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
bf12adbba621223d3feca21c5b95fc7ec55684e22bc36f75ac8bba03ce37ea71
212bb5eaccca98121639811e71e750c4cbfba99e07094c3a0cf2d1400ec85f5f
S=[PH](Oc1ccccc1)Oc1ccccc1
Cl-[P;H0;D4;+0:1](-Cl)(-[Cl;D1;H0:2])=[S;D1;H0:3].[C;D1;H3:4]-[CH;D3;+0:5](-[CH3;D1;+0:6])-[c:7](:[c:8]):[c:9](-[OH;D1;+0:10]):[c:11]>>[C;D1;H3:4]-[CH;D3;+0:5](-[C;D1;H3:12])-[c:7](:[c:8]):[c:9](-[O;H0;D2;+0:10]-[P;H0;D4;+0:1](-[Cl;D1;H0:2])(=[S;D1;H0:3])-[#8:13]-[c:14]:[c:15]:[c:16](-[CH3;D1;+0:6]):[c:17]):[c:11]
63
[{"value": 63.0, "product": "P(=S)(OC1=C(C=CC(=C1)C)C(C)C)(OC1=C(C=CC(=C1)C)C(C)C)Cl", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
2-isopropyl-5-methylphenol was reacted with sodium hydride and thiophosphoryl chloride using the procedure of Example 21 to form bis(2-isopropyl-5-methylphenyl) chlorothiophosphate (31PNMR, singlet, 57 ppm). This compound was reacted with diphenylphosphonothioic amide by the General Method C(ii) (THF) yielding the comp...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
null
null
c1ccccc1
c1ccccc1.c1ccccc1
null
null
null
null
Cc1ccc(C(C)C)c(O)c1.S=P(Cl)(Cl)Cl>>Cc1ccc(C(C)C)c(OP(=S)(Cl)Oc2cc(C)ccc2C(C)C)c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-49348a03da5449a3a6fa1f38365b6d60
CC(=O)Cl.Cc1ccc2c(C(C)CCO)ccc(C(C)C)cc1-2>>CC(=O)OCCC(C)c1ccc(C(C)C)cc2c(C)ccc1-2
C(C)(=O)Cl.C(C)(C)C1=CC=C(C2=CC=C(C2=C1)C)C(CCO)C.N1=CC=CC=C1>>C(C)(=O)OCCC(C)C=1C2=CC=C(C2=CC(=CC1)C(C)C)C
Cl[C:2]([CH3:1])=[O:3].[OH:4][CH2:5][CH2:6][CH:7]([CH3:8])[c:9]1[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][c:17]2[c:18]([CH3:19])[cH:20][cH:21][c:22]1-2>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][CH2:6][CH:7]([CH3:8])[c:9]1[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][c:17]2[c:18]([CH3:19])[cH:20][cH:21][c:...
CC(=O)Cl.Cc1ccc2c(C(C)CCO)ccc(C(C)C)cc1-2
CC(=O)OCCC(C)c1ccc(C(C)C)cc2c(C)ccc1-2
null
null
ClCCl
Acylation
Schotten-Baumann to ester
6cefe709828c5bd4655f254e75d5dff9e8876e192e7dd47256c1bc0067bc5291
d8a7643b81ed07a6f633aa99465180dfa0565e61ae25aef36338ebb9837c9cef
c1ccc2cccc-2cc1
Cl-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[C:4]-[C:5]-[OH;D1;+0:6]>>[C:4]-[C:5]-[O;H0;D2;+0:6]-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3]
null
[]
null
null
1
HOUR
4.8 g (0.063 mol) of acetyl chloride in 20 ml of dichloromethane were added dropwise at 0° C. to a solution of 12.1 g (0.05 mol) of 3-(7-isopropyl-1-methylazulen-4-yl)butanol and 7.9 g (0.1 mol) of pyridine in 100 ml of dichloromethane, and the mixture was stirred at room temperature for 1 hour. It was then extracted w...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary alcohol
Ester
null
null
c1ccc2cccc2cc1
HCl
ClCCl
null
1
CC(=O)Cl.Cc1ccc2c(C(C)CCO)ccc(C(C)C)cc1-2>ClCCl>CC(=O)OCCC(C)c1ccc(C(C)C)cc2c(C)ccc1-2
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f7d58edbb5e54cc089f19cc68f88af86
C/C=C/C(=O)Cl.CCN(CC)CC.Cc1ccc2c(C(C)CCO)ccc(CC(C)C)cc1-2>>C=CCCC(=O)OCCC(C)c1ccc(CC(C)C)cc2c(C)ccc1-2
O.C(\C=C\C)(=O)Cl.C(C(C)C)C1=CC=C(C2=CC=C(C2=C1)C)C(CCO)C.C(C)N(CC)CC>>C(CC=C)C(=O)OCCC(C)C=1C2=CC=C(C2=CC(=CC1)CC(C)C)C
Cl[C:5](/[CH:4]=[CH:3]/[CH3:2])=[O:6].CCN(CC)C[CH3:1].[OH:7][CH2:8][CH2:9][CH:10]([CH3:11])[c:12]1[cH:13][cH:14][c:15]([CH2:16][CH:17]([CH3:18])[CH3:19])[cH:20][c:21]2[c:22]([CH3:23])[cH:24][cH:25][c:26]1-2>>[CH2:1]=[CH:2][CH2:3][CH2:4][C:5](=[O:6])[O:7][CH2:8][CH2:9][CH:10]([CH3:11])[c:12]1[cH:13][cH:14][c:15]([CH2:16...
C/C=C/C(=O)Cl.CCN(CC)CC.Cc1ccc2c(C(C)CCO)ccc(CC(C)C)cc1-2
C=CCCC(=O)OCCC(C)c1ccc(CC(C)C)cc2c(C)ccc1-2
null
null
O1CCCC1
Acylation
OtherReaction
342207de4c335b59324a35212f1f158240c295dd2d150892d3db08d21b0f5356
40fdba0dae1a5a857a281d8885f2ac044c84690ddfd78f39e9253756e50a80a4
c1ccc2cccc-2cc1
C-C-N(-C-C)-C-[CH3;D1;+0:1].Cl-[C;H0;D3;+0:2](=[O;D1;H0:3])/[CH;D2;+0:4]=[CH;D2;+0:5]/[CH3;D1;+0:6].[C:7]-[C:8]-[OH;D1;+0:9]>>[C:7]-[C:8]-[O;H0;D2;+0:9]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[CH2;D2;+0:4]-[CH2;D2;+0:5]-[CH;D2;+0:6]=[CH2;D1;+0:1]
null
[]
null
null
2
HOUR
10.0 g (0.07 mol) of crotonyl chloride were added dropwise at room temperature to a solution of 7.26 g (0.03 mol) of 3-(7-isobutyl-1-methylazulen-4-yl)butanol and 30 ml of triethylamine in 100 ml of tetrahydrofuran, and the mixture was stirred for 2 hours. 50 ml of water were then added, and the batch was thoroughly st...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary alcohol.Tertiary amine
Ester.Allyl
null
null
c1ccc2cccc2cc1
HCl
O1CCCC1
null
2
C/C=C/C(=O)Cl.CCN(CC)CC.Cc1ccc2c(C(C)CCO)ccc(CC(C)C)cc1-2>O1CCCC1>C=CCCC(=O)OCCC(C)c1ccc(CC(C)C)cc2c(C)ccc1-2
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d7d6fec5e6d54cc5b295691760de5f99
CC(=O)OC(C)C(=O)N1c2ccccc2C(C)CC1(C)C>>CC1CC(C)(C)c2cccc(N)c21
N.C(C)(=O)[O-].C(C)(=O)OC(C(=O)N1C(CC(C2=CC=CC=C12)C)(C)C)C.OS(=O)(=O)O>>NC1=C2C(CC(C2=CC=C1)(C)C)C
CC(=O)OC(C)C(=O)[N:12]1[C:4]([CH3:5])([CH3:6])[CH2:3][CH:2]([CH3:1])[c:13]2[cH:7][cH:8][cH:9][cH:10][c:11]21>>[CH3:1][CH:2]1[CH2:3][C:4]([CH3:5])([CH3:6])[c:7]2[cH:8][cH:9][cH:10][c:11]([NH2:12])[c:13]21
CC(=O)OC(C)C(=O)N1c2ccccc2C(C)CC1(C)C
CC1CC(C)(C)c2cccc(N)c21
null
null
C(C)(=O)O.O
Functional Group Interconversion
OtherReaction
751b997eceb2879c79880df7df2a573ebf671ecfbfe066920fb5ebb1bc6a5f31
63989af454af4021ebf3b6c605c13acad5bf9e2283cf20379910b86126ac543d
c1ccc2c(c1)CCC2
C-C(-O-C(-C)=O)-C(=O)-[N;H0;D3;+0:1]1-[c:2]2:[c:3]:[c:4]:[c:5]:[cH;D2;+0:6]:[c:7]:2-[C:8]-[C:9]-[C;H0;D4;+0:10]-1(-[C;D1;H3:11])-[C;D1;H3:12]>>[C;D1;H3:11]-[C;H0;D4;+0:10]1(-[C;D1;H3:12])-[C:9]-[C:8]-[c:7]2:[c:2](-[NH2;D1;+0:1]):[c:3]:[c:4]:[c:5]:[c;H0;D3;+0:6]:2-1
75
[{"value": 69.0, "product": "NC1=C2C(CC(C2=CC=C1)(C)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.0, "product": "NC1=C2C(CC(C2=CC=C1)(C)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
30
MINUTE
The acetate compound prepared in B (ii) (55 g, GC purity 91%, 0.172 moles) was added over 45 minutes to 98% H2SO4 (50 ml) at 25°-60° C. (exotherm). After stirring for a further 30 minutes at 60° C., water (50 ml) containing acetic acid (10 ml) was cautiously added dropwise and the mixture heated at 100° C. for 3 hours....
10.6084/m9.figshare.5104873.v1
null
Ester.Tertiary amide
Primary amine
c1ccc2c(c1)CCC[NH]2
c1ccc2c(c1)CCC2
c1ccc2c(c1)CCC2
HO-
C(C)(=O)O.O
60
0.5
CC(=O)OC(C)C(=O)N1c2ccccc2C(C)CC1(C)C>C(C)(=O)O.O>CC1CC(C)(C)c2cccc(N)c21
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5330fe2873fa4dd296b870c5f2f16b19
CCCCC[C@H]1[C@@H](CC(=O)O)CC[C@H]1O>>CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O
O[C@H]1[C@H]([C@H](CC1)CC(=O)O)CCCCC.[N+](=[N-])=C>>O[C@H]1[C@H]([C@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C@@H:7]([CH2:8][C:9](=[O:10])[OH:11])[CH2:13][CH2:14][C@H:15]1[OH:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C@@H:7]([CH2:8][C:9](=[O:10])[O:11][CH3:12])[CH2:13][CH2:14][C@H:15]1[OH:16]
CCCCC[C@H]1[C@@H](CC(=O)O)CC[C@H]1O
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O
null
null
CCOCC
Miscellaneous
OtherReaction
56520e0abb4535dce9a663824ca803b71c2c0dd72dfd246317d953596a987bd2
2ccc7a30191c2c171b49e8a0217bee87430687dd0f567141eca025a75b7e3136
C1CCCC1
[C:1]-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4]>>[C:1]-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-[C;D1;H3:5]
null
[]
null
null
null
null
It is to be noted that (+)-(1R,2S,3R)-3-hydroxy-2-pentyl-1-cyclopentaneacetic acid, used as starting product in this variant of the process of the invention, can also be directly methylated, for example by reacting it with an excess of diazomethane in ether solution, to provide pratically pure methyl (+)-(1R,2S,3R)-3-h...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
C1CCCC1
Other
CCOCC
null
null
CCCCC[C@H]1[C@@H](CC(=O)O)CC[C@H]1O>CCOCC>CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9351ff791ece43d89068d7c5e43ad1d4
CCO.CCO.C[C@H](N)c1ccccc1.O=C(O)C(O)C(O)C(=O)O>>CCCCC[C@H]1[C@@H](CC(=O)O)CC[C@H]1O.CCCCC[C@H]1[C@@H](CC(=O)[O-])CC[C@H]1O.C[C@H]([NH3+])c1ccccc1
C1(=CC=CC=C1)[C@H](C)N.C(C)O.C(C)O.C(C(C(=O)O)O)(C(=O)O)O>>O[C@H]1[C@H]([C@H](CC1)CC(=O)[O-])CCCCC.C1(=CC=CC=C1)[C@H](C)[NH3+].O[C@H]1[C@H]([C@H](CC1)CC(=O)O)CCCCC
O[CH2:19][CH3:20].[CH3:16][CH2:17][OH:30].[CH3:31][C@H:32]([NH2:33])[c:34]1[cH:35][cH:36][cH:37][cH:38][cH:39]1.O[CH:3]([CH:2]([C:1](=[O:10])[OH:11])[OH:15])[C:24](=[O:25])[OH:26]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C@@H:7]([CH2:8][C:9](=[O:10])[OH:11])[CH2:12][CH2:13][C@H:14]1[OH:15].[CH3:16][CH2:17][CH2:18][...
CCO.CCO.C[C@H](N)c1ccccc1.O=C(O)C(O)C(O)C(=O)O
CCCCC[C@H]1[C@@H](CC(=O)O)CC[C@H]1O.CCCCC[C@H]1[C@@H](CC(=O)[O-])CC[C@H]1O.C[C@H]([NH3+])c1ccccc1
null
null
null
Acylation
OtherReaction
de2ad0bd7c39560a69b3b3d1fe2cfe0e1edce6eb87dd7e51b82c0953a8dd5326
feccad8295f640ff4fd9de21f05c157d1cf018b16fa25ae9bb222c8953cc88e2
C1CCCC1.C1CCCC1.c1ccccc1
O-[CH2;D2;+0:1]-[CH3;D1;+0:2].O-[CH;D3;+0:3](-[C;H0;D3;+0:4](=[O;D1;H0:5])-[OH;D1;+0:6])-[CH;D3;+0:7](-[OH;D1;+0:8])-[C;H0;D3;+0:9](=[O;H0;D1;+0:10])-[OH;D1;+0:11].[C;D1;H3:12]-[CH2;D2;+0:13]-[OH;D1;+0:14].[C;D1;H3:15]-[C:16](-[NH2;D1;+0:17])-[c:18]>>[C;D1;H3:15]-[C:16](-[NH3+;D1:17])-[c:18].[C:19]-[C:20](-[OH;D1;+0:14...
null
[]
null
null
null
null
This acid presented the analytical characters of the racemic acid described under b) and a [α]20D =-12° (c=1.15, ethanol) (purity: 99%; e.r. 99.2:0.8). Proceeding in a manner analogous to that described here-above, but using (-)-(S)-1-penylethylamine (Fluka purum; e.r. 98:2), there was obtained (1R,2S,3R)-3-hydroxy-2-p...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Carboxylic acid.Primary alcohol.Primary alcohol.Secondary alcohol.Secondary alcohol.Primary amine
Carboxylic acid.Secondary alcohol.Secondary alcohol
null
C1CCCC1.C1CCCC1
C1CCCC1.C1CCCC1.c1ccccc1
null
null
null
null
CCO.CCO.C[C@H](N)c1ccccc1.O=C(O)C(O)C(O)C(=O)O>>CCCCC[C@H]1[C@@H](CC(=O)O)CC[C@H]1O.CCCCC[C@H]1[C@@H](CC(=O)[O-])CC[C@H]1O.C[C@H]([NH3+])c1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-a0652456c8c14b52877012b598e65bcc
CCCCCC1=C(CC(=O)O)CCC1=O>>CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)O
O=C1C(=C(CC1)CC(=O)O)CCCCC.C(Cl)Cl.C(C)N(CC)CC>>O=C1[C@H]([C@H](CC1)CC(=O)O)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]1=[C:11]([CH2:12][C:13](=[O:14])[OH:15])[CH2:10][CH2:9][C:7]1=[O:8]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@@H:11]1[CH2:12][C:13](=[O:14])[OH:15]
CCCCCC1=C(CC(=O)O)CCC1=O
CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)O
null
null
CO
Reduction
Hydrogenation (double to single)
86ab11674f5c386e6bf85e3207d59c3e1c24536199ef80ba4c93b215304815db
0e0db21233797ec1d2a9464a1f32cef94e53e6a41f96d680fa1307067bbf01f2
O=C1CCCC1
[C:1]-[C:2]-[C;H0;D3;+0:3]1=[C;H0;D3;+0:4](-[C:5]-[C:6](=[O;D1;H0:7])-[O;D1;H1:8])-[C:9]-[C:10]-[C:11]-1=[O;D1;H0:12]>>[C:1]-[C:2]-[C@@H;D3;+0:3]1-[C:11](=[O;D1;H0:12])-[C:10]-[C:9]-[C@@H;D3;+0:4]-1-[C:5]-[C:6](=[O;D1;H0:7])-[O;D1;H1:8]
null
[]
null
null
5
MINUTE
Into a Schlenk type vessel, kept anhydrous and under Ar, there was injected the precatalytic solution (6.75 ml) containing 47 mg (0.05 mmole) of bis(trifluoro-acetato)[(+)-(R)-2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl]ruthenium (II), 3-oxo-2-pentyl-1-cyclopentene-1-acetic acid (0.5 g, 2.4 mmole), CH2Cl2 (5 ml), meth...
10.6084/m9.figshare.5104873.v1
null
Ketone
Ketone
C1=CCCC1
C1CCCC1
C1CCCC1
null
CO
null
0.083333
CCCCCC1=C(CC(=O)O)CCC1=O>CO>CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5e5ea1bad7f34a958fa0ed6555062f7d
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O>>CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)OC
O[C@H]1[C@H]([C@H](CC1)CC(=O)OC)CCCCC.C=1C=C[NH+]=CC1.[O-][Cr](=O)(=O)Cl.C(C)(=O)[O-].[Na+]>>O=C1[C@H]([C@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@@H:6]1[C@H:7]([OH:8])[CH2:9][CH2:10][C@@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O
CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)OC
null
null
null
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
6ad3a11b438c0e1c50a70c6d16bbab7d61c75949455edc72e81522617519349d
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C1CCCC1
[C:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[C@H;D3;+0:6]-1-[OH;D1;+0:7]>>[C:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[C;H0;D3;+0:6]-1=[O;H0;D1;+0:7]
94.9
[{"value": 92.7, "product": "O=C1[C@H]([C@H](CC1)CC(=O)OC)CCCCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 94.9, "product": "O=C1[C@H]([C@H](CC1)CC(=O)OC)CCCCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
This ester (2.85 g) was then oxidized by means of PCC, in the presence of sodium acetate, in a manner analogous to the method described in Example 1 d), to yield 2.68 g of the desired methyl (+)-(1R)-cis-3-oxo-2-pentyl-1-cyclopentaneacetate (colorless oil; purity 98.5%; yield 92.7%). Conditions: See reaction.notes.proc...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
C1CCCC1
C1CCCC1
C1CCCC1
null
null
null
null
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O>>CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4de432ae17d04f5487e4f075f169e736
CCCCC[C@@H]1[C@H](CC(=O)OC)CC[C@@H]1O>>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
O[C@@H]1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC>>O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C@@H:7]([OH:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CCCCC[C@@H]1[C@H](CC(=O)OC)CC[C@@H]1O
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
null
null
CO
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
6ad3a11b438c0e1c50a70c6d16bbab7d61c75949455edc72e81522617519349d
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C1CCCC1
[C:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[C@@H;D3;+0:6]-1-[OH;D1;+0:7]>>[C:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[C;H0;D3;+0:6]-1=[O;H0;D1;+0:7]
null
[]
null
null
null
null
The intermediate methyl (-)-(1S,2R,3S)-3-hydroxy-2-pentyl-1-cyclopentane acetate presented a [α]20D =-16° (c=1.805, methanol) Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
C1CCCC1
C1CCCC1
C1CCCC1
null
CO
null
null
CCCCC[C@@H]1[C@H](CC(=O)OC)CC[C@@H]1O>CO>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c559e57f319541fc972edd30a8da1304
CCCCCC1=C(CC(=O)O)CCC1=O.CCN(CC)CC>>CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)OC
O=C1C(=C(CC1)CC(=O)O)CCCCC.C(C)N(CC)CC.[H][H]>>O=C1[C@H]([C@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]1=[C:11]([CH2:12][C:13](=[O:14])[OH:15])[CH2:10][CH2:9][C:7]1=[O:8].CCN(CC)C[CH3:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CCCCCC1=C(CC(=O)O)CCC1=O.CCN(CC)CC
CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)OC
null
null
C1CCOC1.CO
Heteroatom Alkylation and Arylation
OtherReaction
da196e3236d736556fdcfb1837b2770790986d12ec118891fa08f19c2fb48760
1780374e34072fe6cc492484130d27a3000ef633f8afc7bcab57f8989bcf035e
O=C1CCCC1
C-C-N(-C-C)-C-[CH3;D1;+0:1].[C:2]-[C:3]-[C;H0;D3;+0:4]1=[C;H0;D3;+0:5](-[C:6]-[C:7](=[O;D1;H0:8])-[OH;D1;+0:9])-[C:10]-[C:11]-[C:12]-1=[O;D1;H0:13]>>[C:2]-[C:3]-[C@@H;D3;+0:4]1-[C:12](=[O;D1;H0:13])-[C:11]-[C:10]-[C@@H;D3;+0:5]-1-[C:6]-[C:7](=[O;D1;H0:8])-[O;H0;D2;+0:9]-[CH3;D1;+0:1]
null
[]
null
null
4
HOUR
To a solution of 252 mg (1.20 mmole) 3-oxo-2-pentyl-1 cyclopentene-1-acetic acid, in a mixture of 7 ml of THF and 21 ml of methanol, there were added 2 ml of the catalyst solution obtained in a) (0.025 mmole, 0.021 eq.) and 10.4 μl of triethylamine (0.075 mmole, 3 eq.) under stirring at r.t. This solution, prepared in ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ketone.Tertiary amine
Ketone.Ester
C1=CCCC1
C1CCCC1
C1CCCC1
Other
C1CCOC1.CO
null
4
CCCCCC1=C(CC(=O)O)CCC1=O.CCN(CC)CC>C1CCOC1.CO>CCCCC[C@@H]1C(=O)CC[C@@H]1CC(=O)OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-13f0bb09496b4e76add90df9bebc924b
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)O.COC(=O)OC(=O)OC>>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
O=C1[C@@H]([C@@H](CC1)CC(=O)O)CCCCC.C(=O)(OC)OC(=O)OC>>O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[OH:15].COC(=O)OC(=O)O[CH3:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)O.COC(=O)OC(=O)OC
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
null
null
CO
Heteroatom Alkylation and Arylation
O-methylation
ab70ccb44fd2770c6bb4cd50876c98fd63fd5433f67c38378b2c3cf9fd8e3bb7
98c84e009887ebe0ace192c2ccbdd6041fa48ce8e27f6f302e5a3939fc247f0b
O=C1CCCC1
C-O-C(=O)-O-C(=O)-O-[CH3;D1;+0:1].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
90
[{"value": 90.0, "product": "O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
104 Mg (0.49 mmole) of (+)-cis-3-oxo-2-pentyl-1-cyclopentaneacetic acid (97:3 cis/trans ratio) in 0.5 ml of methanol were treated with 76 μl of dimethyl dicarbonate [CH3O(CO)O(CO)OCH3, origin: Bayer; 96 mg, 0.72 mmole, 1.5 eq.]. The resulting solution was heated to 45° during 16 h and then evaporated under vacuum. Afte...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Carbonic Ester.Carbonic Ester.Carboxylic acid
Ester
null
null
C1CCCC1
HO-
CO
null
null
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)O.COC(=O)OC(=O)OC>CO>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-cb6326117e3045cb93e4c9a0471e9b58
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)O.COS(=O)(=O)OC>>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
CCOCC.COS(=O)(=O)OC.O=C1[C@@H]([C@@H](CC1)CC(=O)O)CCCCC>>O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[OH:15].COS(=O)(=O)O[CH3:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)O.COS(=O)(=O)OC
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
null
null
O.CC(=O)C
Heteroatom Alkylation and Arylation
Methylation of OH with DMS
9474aa79a2adc7353c0c02444ca598a6f486ecdd7ed5edb9ae0645721ee50389
badd4f82161bb0ee7acffd023ea4caae5d036bce7065c10ab0a06e83a6a6f119
O=C1CCCC1
C-O-S(=O)(=O)-O-[CH3;D1;+0:1].[C:2]-[C:3](=[O;D1;H0:4])-[OH;D1;+0:5]>>[C:2]-[C:3](=[O;D1;H0:4])-[O;H0;D2;+0:5]-[CH3;D1;+0:1]
89.8
[{"value": 84.0, "product": "O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 89.8, "product": "O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To 104 mg (0.49 mmole) of (±)cis-3-oxo-2-pentyl-1-cyclopentaneacetic acid (93:7 cis/trans ratio) in 1 ml of (CH3)2CO there were added, first 56 μl of (CH3)2SO4 (74 ml, 0.59 mmole, 1.2 eq.) and then 81 mg (0.59 mmole, 1.2 eq.) of anhydrous solid K2 CO3. The resulting suspension was heated at r.t. during 4 h and taken in...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ester
null
null
C1CCCC1
HO-
O.CC(=O)C
null
null
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)O.COS(=O)(=O)OC>O.CC(=O)C>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-796c9df1b95145c8a5bab3faf51eb692
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O>>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
O[C@H]1[C@H]([C@H](CC1)CC(=O)OC)CCCCC>>O=C1[C@@H]([C@@H](CC1)CC(=O)OC)CCCCC
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@@H:6]1[C@H:7]([OH:8])[CH2:9][CH2:10][C@@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][C@H:6]1[C:7](=[O:8])[CH2:9][CH2:10][C@H:11]1[CH2:12][C:13](=[O:14])[O:15][CH3:16]
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O
CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
null
null
CO
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
6ad3a11b438c0e1c50a70c6d16bbab7d61c75949455edc72e81522617519349d
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C1CCCC1
[C:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[C@H;D3;+0:6]-1-[OH;D1;+0:7]>>[C:1]-[C:2]1-[C:3]-[C:4]-[C:5]-[C;H0;D3;+0:6]-1=[O;H0;D1;+0:7]
null
[]
null
null
null
null
methyl (+)-(1R,2S,3R)-3-hydroxy-2-pentyl-1-cyclopentaneacetate, characterized by a [α]20D superior to +17° (c=1.795 g/ 100 ml, methanol). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
C1CCCC1
C1CCCC1
C1CCCC1
null
CO
null
null
CCCCC[C@H]1[C@@H](CC(=O)OC)CC[C@H]1O>CO>CCCCC[C@H]1C(=O)CC[C@H]1CC(=O)OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d6f1159968164ca59973a165fcea56a0
COC(=O)c1ccc2cc(C(=O)OC)ccc2c1>>O=C(O)c1ccc2cc(C(=O)O)ccc2c1
COC(=O)C1=CC2=CC=C(C=C2C=C1)C(=O)OC.COC(=O)C1=CC2=CC=C(C=C2C=C1)C(=O)OC>>C1=C(C=CC2=CC(=CC=C12)C(=O)O)C(=O)O
C[O:3][C:2](=[O:1])[c:4]1[cH:5][cH:6][c:7]2[cH:8][c:9]([C:10](=[O:11])[O:12]C)[cH:13][cH:14][c:15]2[cH:16]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]2[cH:8][c:9]([C:10](=[O:11])[OH:12])[cH:13][cH:14][c:15]2[cH:16]1
COC(=O)c1ccc2cc(C(=O)OC)ccc2c1
O=C(O)c1ccc2cc(C(=O)O)ccc2c1
null
[Cr].[Co]
null
Deprotection
OtherReaction
6e62db7aac546f574bcfb83067ba8906c30fcbfedfc37aa16b5eaad33833f45a
ed5fed81ba501ef41c88831ec6b9463b899bfdd0815c4145ae51c79addb226d0
c1ccc2ccccc2c1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].C-[O;H0;D2;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4].[O;D1;H0:7]=[C:6](-[OH;D1;+0:5])-[c:8]
null
[]
null
null
null
null
Dimethyl-2,6-naphthalenedicarboxylate was hydrolyzed at elevated temperatures and elevated pressures in the batch-mode in a stirred, 300 ml Hastelloy C autoclave reactor. 37.5 Grams of dimethyl-2,6-naphthalenedicarboxylate were charged to the reactor. No catalyst was used. The 2,6-NDA product was separated from the mot...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Carboxylic acid.Carboxylic acid
null
null
c1ccc2ccccc2c1
Other
[Cr].[Co]
null
null
COC(=O)c1ccc2cc(C(=O)OC)ccc2c1>[Cr].[Co]>O=C(O)c1ccc2cc(C(=O)O)ccc2c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-558175fef481481a9e6bb6eb3ef92dfd
COC(=O)c1ccc2cc(C(=O)OC)ccc2c1>>O=C(O)c1ccc2cc(C(=O)O)ccc2c1
COC(=O)C1=CC2=CC=C(C=C2C=C1)C(=O)OC>>C1=C(C=CC2=CC(=CC=C12)C(=O)O)C(=O)O
C[O:3][C:2](=[O:1])[c:4]1[cH:5][cH:6][c:7]2[cH:8][c:9]([C:10](=[O:11])[O:12]C)[cH:13][cH:14][c:15]2[cH:16]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][cH:6][c:7]2[cH:8][c:9]([C:10](=[O:11])[OH:12])[cH:13][cH:14][c:15]2[cH:16]1
COC(=O)c1ccc2cc(C(=O)OC)ccc2c1
O=C(O)c1ccc2cc(C(=O)O)ccc2c1
null
[Ti]
null
Deprotection
OtherReaction
6e62db7aac546f574bcfb83067ba8906c30fcbfedfc37aa16b5eaad33833f45a
ed5fed81ba501ef41c88831ec6b9463b899bfdd0815c4145ae51c79addb226d0
c1ccc2ccccc2c1
C-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].C-[O;H0;D2;+0:5]-[C:6](=[O;D1;H0:7])-[c:8]>>[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4].[O;D1;H0:7]=[C:6](-[OH;D1;+0:5])-[c:8]
null
[]
null
null
null
null
The hydrolysis of dimethyl-2,6-naphthalenedicarboxylate was conducted in the batch-mode in a 2 liter, stirred, titanium-lined reactor. The reaction time, temperature, pressure and analysis of the resulting 2,6-naphthalenedicarboxylic acid are provided in Table 5. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ester.Ester
Carboxylic acid.Carboxylic acid
null
null
c1ccc2ccccc2c1
Other
[Ti]
null
null
COC(=O)c1ccc2cc(C(=O)OC)ccc2c1>[Ti]>O=C(O)c1ccc2cc(C(=O)O)ccc2c1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-82f26f3da9b94277b41d5e2a0b568816
O=[N+]([O-])c1ccccc1S(=O)(=O)Cl.[OH-].[OH-]>>Nc1ccc(-c2ccc(N)c(S(=O)(=O)O)c2)cc1S(=O)(=O)O
Cl.[N+](=O)([O-])C1=C(C=CC=C1)S(=O)(=O)Cl.[OH-].[Na+].[OH-].[Na+]>>NC1=C(C=C(C=C1)C1=CC(=C(C=C1)N)S(=O)(=O)O)S(=O)(=O)O
Cl[S:12]([c:11]1[c:9]([N+:1]([O-:15])=[O:21])[cH:2][cH:5][cH:6][cH:16]1)(=[O:13])=[O:14].[OH-:20].[OH-:22]>>[NH2:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[cH:7][cH:8][c:9]([NH2:10])[c:11]([S:12](=[O:13])(=[O:14])[OH:15])[cH:16]2)[cH:17][c:18]1[S:19](=[O:20])(=[O:21])[OH:22]
O=[N+]([O-])c1ccccc1S(=O)(=O)Cl.[OH-].[OH-]
Nc1ccc(-c2ccc(N)c(S(=O)(=O)O)c2)cc1S(=O)(=O)O
null
[Zn]
null
Aromatic Heterocycle Formation
OtherReaction
2ddb7c090d049d9b01b596b1c5531306ec590605e5521218aaf87a1a76a70d6e
b985031033afe35c77179a62d23d1deb378f8cb143d9567147a092876a6f49a9
c1ccc(-c2ccccc2)cc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4]1:[c:5]:[cH;D2;+0:6]:[cH;D2;+0:7]:[cH;D2;+0:8]:[c;H0;D3;+0:9]:1-[N+;H0;D3:10](-[O-;H0;D1:11])=[O;H0;D1;+0:12].[OH-;D0:13].[OH-;D0:14]>>[N;D1;H2:15]-[c;H0;D3;+0:9]1:[c:16]:[c:17]:[c;H0;D3;+0:6](-[c;H0;D3;+0:7]2:[c:18]:[c:19](-[#16:20](=[O;H0;D1;+0:13])(=[O;H0;D1;+0:12])...
28.6
[{"value": 28.6, "product": "NC1=C(C=C(C=C1)C1=CC(=C(C=C1)N)S(=O)(=O)O)S(=O)(=O)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 25.2, "product": "NC1=C(C=C(C=C1)C1=CC(=C(C=C1)N)S(=O)(=O)O)S(=O)(=O)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
1
HOUR
A 500 mL flask equipped with mechanical stirrer, condenser, addition funnel, and thermometer was charged with 50.0 g (0.255 mol) of 2-nitrobenzene sulfonyl chloride (Aldrich). Upon dropwise addition of 5M aqueous sodium hydroxide (125 mL, 0.625 mol) the reaction mixture warmed to 80° C. and a dark red/brown solution re...
10.6084/m9.figshare.5104873.v1
null
Nitro group.Sulfonyl halide
Primary amine.Primary amine.Sulfonic acid.Sulfonic acid
c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
null
[Zn]
80
1
O=[N+]([O-])c1ccccc1S(=O)(=O)Cl.[OH-].[OH-]>[Zn]>Nc1ccc(-c2ccc(N)c(S(=O)(=O)O)c2)cc1S(=O)(=O)O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-07ac67ae638344aebabaeb810563c749
O=C(NC(CO)CO)c1c(I)c(O)c(I)c(C(=O)NC(CO)CO)c1I>>C[C@H](Oc1c(I)c(C(=O)NC(CO)CO)c(I)c(C(=O)NC(CO)CO)c1I)C(N)=O
[Na].OCC(CO)NC(=O)C1=C(C(=C(C(=C1I)O)I)C(=O)NC(CO)CO)I>>NC([C@@H](OC=1C(=C(C(=C(C1I)C(=O)NC(CO)CO)I)C(=O)NC(CO)CO)I)C)=O
[CH2:1]([CH:22]([NH:21][C:19]([c:18]1[c:16]([I:17])[c:7]([C:8](=[O:9])[NH:10][CH:11]([CH2:12][OH:13])[CH2:14][OH:15])[c:5]([I:6])[c:4]([OH:3])[c:27]1[I:28])=[O:20])[CH2:29][OH:31])[OH:24]>>[CH3:1][C@H:2]([O:3][c:4]1[c:5]([I:6])[c:7]([C:8](=[O:9])[NH:10][CH:11]([CH2:12][OH:13])[CH2:14][OH:15])[c:16]([I:17])[c:18]([C:19]...
O=C(NC(CO)CO)c1c(I)c(O)c(I)c(C(=O)NC(CO)CO)c1I
C[C@H](Oc1c(I)c(C(=O)NC(CO)CO)c(I)c(C(=O)NC(CO)CO)c1I)C(N)=O
null
null
COCCO
Miscellaneous
OtherReaction
6c8f2b3bb952a7fe9d9ba1794c21b2ecbef479b16f5b4683569e954e672b1596
7e4dda57e0c86b8a383110aab23b72da24ab712be2c6b3824e86a807871fa757
c1ccccc1
[O;D1;H0:1]=[C:2](-[#7:3]-[CH;D3;+0:4](-[CH2;D2;+0:5]-[OH;D1;+0:6])-[CH2;D2;+0:7]-[OH;D1;+0:8])-[c:9]:[c:10]:[c:11](-[OH;D1;+0:12]):[c:13]>>[CH3;D1;+0:5]-[C:14](-[O;H0;D2;+0:12]-[c:11](:[c:13]):[c:10]:[c:9]-[C:2](=[O;D1;H0:1])-[#7:3]-[CH;D3;+0:4](-[C:15]-[OH;D1;+0:6])-[C:16]-[O;D1;H1:17])-[C;H0;D3;+0:7](-[N;D1;H2:18])=...
90.3
[{"value": 45.0, "product": "NC([C@@H](OC=1C(=C(C(=C(C1I)C(=O)NC(CO)CO)I)C(=O)NC(CO)CO)I)C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.3, "product": "NC([C@@H](OC=1C(=C(C(=C(C1I)C(=O)NC(CO)CO)I)C(=O)NC(CO)CO)I)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
8
HOUR
To a solution of 21.8 g of N,N'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-hydroxy-2,4,6-triiodo-1,3-benzenedicarboxamide sodium salt (prepared according to the procedure described in patent EP 185130) (0.03 mol) in 70 mL of methyl cellosolve, heated to 80° C., 14.6 g of R-2-[[(4-methylphenyl)sulfonyl]oxy]propanamide (pre...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Primary alcohol.Aromatic alcohol
Ether.Primary amide.Primary alcohol.Primary alcohol
null
null
c1ccccc1
Other
COCCO
80
8
O=C(NC(CO)CO)c1c(I)c(O)c(I)c(C(=O)NC(CO)CO)c1I>COCCO>C[C@H](Oc1c(I)c(C(=O)NC(CO)CO)c(I)c(C(=O)NC(CO)CO)c1I)C(N)=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-5d0de86ea40e4c07a7ac73d256823ecf
C=CN(C=O)CCC(=O)OC.OCCNCCO>>C=CN(C=O)CCC(=O)N(CCO)CCO
C(=C)N(C=O)CCC(=O)OC.N(CCO)CCO.C[O-].[Na+]>>OCCN(C(CCN(C=O)C=C)=O)CCO
CO[C:8]([CH2:7][CH2:6][N:3]([CH:2]=[CH2:1])[CH:4]=[O:5])=[O:9].[NH:10]([CH2:11][CH2:12][OH:13])[CH2:14][CH2:15][OH:16]>>[CH2:1]=[CH:2][N:3]([CH:4]=[O:5])[CH2:6][CH2:7][C:8](=[O:9])[N:10]([CH2:11][CH2:12][OH:13])[CH2:14][CH2:15][OH:16]
C=CN(C=O)CCC(=O)OC.OCCNCCO
C=CN(C=O)CCC(=O)N(CCO)CCO
null
null
CO
Acylation
Aminolysis of esters
d147787750807073759132276086de98566af6772417f9288b6300bf1de7801c
fa66342dd118fe5531ba6a998ac8fab92d2b0db4fd04688560eec7d04e9be0e4
null
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C:5]-[C:6]-[NH;D2;+0:7]-[C:8]-[C:9]>>[C:5]-[C:6]-[N;H0;D3;+0:7](-[C:8]-[C:9])-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]
null
[]
90
CELSIUS
2
HOUR
A 50 mL single-neck round bottom flask equipped with a distillation head was charged with 15.1 grams (0.096 mole) of methyl 3-(N-vinylformamido)propionate, 9.95 grams (0.09 mole) of diethanolamine and 0.15 gram of 25% sodium methoxide in methanol solution. The mixture was stirred at 90° C. for 2 hours and the generated...
10.6084/m9.figshare.5104873.v1
null
Ester.Secondary amine
Tertiary amide
null
null
null
HO-
CO
90
2
C=CN(C=O)CCC(=O)OC.OCCNCCO>CO>C=CN(C=O)CCC(=O)N(CCO)CCO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d45c299f3f91429abf2d8013fc0f56fb
C=CN(C=O)CCC(=O)OCC.C[O-].NCCN.NCCN>>C=CN(C=O)CCC(=O)NCCNC(=O)CCN(C=C)C=O
C(CN)N.C(=C)N(C=O)CCC(=O)OCC.C(CN)N.C[O-].[Na+]>>C(=C)N(C=O)CCC(=O)NCCNC(CCN(C=O)C=C)=O
[CH2:1]=[CH:2][N:3]([CH:4]=[O:15])[CH2:6][CH2:7][C:8]([O:5][CH2:19][CH3:20])=[O:9].[CH3:21][O-:22].N[CH2:16][CH2:17][NH2:18].[NH2:10][CH2:11][CH2:14][NH2:13]>>[CH2:1]=[CH:2][N:3]([CH:4]=[O:5])[CH2:6][CH2:7][C:8](=[O:9])[NH:10][CH2:11][CH2:12][NH:13][C:14](=[O:15])[CH2:16][CH2:17][N:18]([CH:19]=[CH2:20])[CH:21]=[O:22]
C=CN(C=O)CCC(=O)OCC.C[O-].NCCN.NCCN
C=CN(C=O)CCC(=O)NCCNC(=O)CCN(C=C)C=O
null
null
CO
C-C Coupling
OtherReaction
62ae3da8cb19b8d040118904bcb1f3a539341fc71d3ddcfc2887e79538c70173
9ec590a7bb0409b1f6b8f9fad2afd2457245fdc91c202c3ff73cfd6ce32440ce
null
N-[CH2;D2;+0:1]-[C:2]-[NH2;D1;+0:3].[C;D1;H2:4]=[C:5]-[#7:6](-[C:7]-[C:8]-[C;H0;D3;+0:9](=[O;D1;H0:10])-[O;H0;D2;+0:11]-[CH2;D2;+0:12]-[CH3;D1;+0:13])-[CH;D2;+0:14]=[O;H0;D1;+0:15].[CH3;D1;+0:16]-[O-;H0;D1:17].[NH2;D1;+0:18]-[CH2;D2;+0:19]-[CH2;D2;+0:20]-[NH2;D1;+0:21]>>[C;D1;H2:4]=[C:5]-[#7:6](-[C:7]-[C:8]-[C;H0;D3;+0...
null
[]
90
CELSIUS
3
HOUR
The apparatus of Example 2 was charged with 17.1 grams (0.1 mole) of ethyl 3-(N-vinylformamido)propionate, 3.0 grams (0.05 mole) of ethylenediamine and 0.12 gram of 25% sodium methoxide in methanol solution. The mixture was stirred at 90° C. for 3 hours, after which the ethanol coproduct was removed by distillation at ...
10.6084/m9.figshare.5104873.v1
null
Ester.Tertiary amide.Primary amine.Primary amine.Primary amine.Primary amine
Enamine.Secondary amide.Secondary amide.Tertiary amide.Tertiary amide
null
null
null
null
CO
90
3
C=CN(C=O)CCC(=O)OCC.C[O-].NCCN.NCCN>CO>C=CN(C=O)CCC(=O)NCCNC(=O)CCN(C=C)C=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-575fdaab9b024e09a2ac34fb099e5fd0
C=CN(C=O)CCC(=O)OC.NCCCCCO>>C=CN(C=O)CCC(=O)NCCCCCO
C(=C)N(C=O)CCC(=O)OC.NCCCCCO.C[O-].[Na+]>>OCCCCCNC(CCN(C=O)C=C)=O
CO[C:8]([CH2:7][CH2:6][N:3]([CH:2]=[CH2:1])[CH:4]=[O:5])=[O:9].[NH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][OH:16]>>[CH2:1]=[CH:2][N:3]([CH:4]=[O:5])[CH2:6][CH2:7][C:8](=[O:9])[NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][OH:16]
C=CN(C=O)CCC(=O)OC.NCCCCCO
C=CN(C=O)CCC(=O)NCCCCCO
null
null
CO
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
null
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]
null
[]
null
null
null
null
The apparatus of Example 2 was charged with 15.7 grams (0.1 mol) of methyl 3-(N-vinylformamido)propionate, 10.3 grams (0.1 mol) of 5-amino-1-pentanol and 0.12 gram of 25% sodium methoxide in methanol solution. The mixture was stirred at 90° C. for 3 hours after which the methanol coproduct was removed by distillation a...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
null
HO-
CO
null
null
C=CN(C=O)CCC(=O)OC.NCCCCCO>CO>C=CN(C=O)CCC(=O)NCCCCCO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9263fd3c38db4e7d8af1acf74087dcb3
C=CN(C=O)CCC(=O)OCC.OCCO>>C=CN(C=O)CCC(=O)OCCO
C(C)O.C(=C)N(C=O)CCC(=O)OCC.C(CO)O.C[O-].[Na+]>>C(=C)N(C=O)CCC(=O)OCCO
CCO[C:8]([CH2:7][CH2:6][N:3]([CH:2]=[CH2:1])[CH:4]=[O:5])=[O:9].[OH:10][CH2:11][CH2:12][OH:13]>>[CH2:1]=[CH:2][N:3]([CH:4]=[O:5])[CH2:6][CH2:7][C:8](=[O:9])[O:10][CH2:11][CH2:12][OH:13]
C=CN(C=O)CCC(=O)OCC.OCCO
C=CN(C=O)CCC(=O)OCCO
null
null
CO
Acylation
Transesterification
c42e047d71ad2593a6d29093d1fe2ca16ccfd6db7b15eecf1eab340181aef83e
cb08be6428b0a3737df44d00995165c06a05fb7dec4fab744c09315c4f7771d4
null
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C:5]-[C:6]-[OH;D1;+0:7]>>[C:5]-[C:6]-[O;H0;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]
null
[]
90
CELSIUS
2
HOUR
The apparatus of Example 2 was charged with 17.1 grams (0.1 mol) of ethyl 3-(N-vinylformamido)propionate, 6.2 grams (0.1 mol) of ethylene glycol, and 0.15 gram of 25% sodium methoxide in methanol solution. The mixture was stirred at 90° C. for 2 hours. No evolution of ethanol was observed during the reaction period. He...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary alcohol
Ester
null
null
null
HO-
CO
90
2
C=CN(C=O)CCC(=O)OCC.OCCO>CO>C=CN(C=O)CCC(=O)OCCO
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-e627c68d0c1743fc987ec32e90fb2b64
C=CCN.C=CN(C=O)CCC(=O)OCC>>C=CCNC(=O)CCN(C=C)C=O
C(=C)N(C=O)CCC(=O)OCC.C(C=C)N.C[O-].[Na+]>>C(C=C)NC(CCN(C=O)C=C)=O
[CH2:1]=[CH:2][CH2:3][NH2:4].CCO[C:5](=[O:6])[CH2:7][CH2:8][N:9]([CH:10]=[CH2:11])[CH:12]=[O:13]>>[CH2:1]=[CH:2][CH2:3][NH:4][C:5](=[O:6])[CH2:7][CH2:8][N:9]([CH:10]=[CH2:11])[CH:12]=[O:13]
C=CCN.C=CN(C=O)CCC(=O)OCC
C=CCNC(=O)CCN(C=C)C=O
null
null
CO
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
null
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C;D1;H2:5]=[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:8]-[C:7]-[C:6]=[C;D1;H2:5]
null
[]
90
CELSIUS
null
null
A 100mL stainless steel high pressure reactor was charged with 17.1 grams (0.1 mol) of ethyl 3-(N-vinylformamido)propionate, 5.7 grams (0.1 mol) of allylamine and 0.15 gram of 25% sodium methoxide in methanol solution. The mixture was heated at 90° C. for 3 hours. Subsequent NMR analysis of the reaction mixture showed ...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
null
HO-
CO
90
null
C=CCN.C=CN(C=O)CCC(=O)OCC>CO>C=CCNC(=O)CCN(C=C)C=O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-355d5064f2ac4906ba01a2625517f872
CN(C)S(=O)(=O)Cl.COc1ccc(CCNC(=O)[C@@H](N)C(C)C)cc1OC>>COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)(=O)N(C)C)cc1OC
Cl.COC=1C=C(C=CC1OC)CCNC([C@H](C(C)C)N)=O.C(C)N(CC)CC.CN(S(=O)(=O)Cl)C>>COC=1C=C(C=CC1OC)CCNC([C@](C(C)C)(S(N(C)C)(=O)=O)N)=O
Cl[S:17](=[O:18])(=[O:19])[N:20]([CH3:21])[CH3:22].[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][NH:9][C:10](=[O:11])[C@@H:12]([NH2:13])[CH:14]([CH3:15])[CH3:16])[cH:23][c:24]1[O:25][CH3:26]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][NH:9][C:10](=[O:11])[C@:12]([NH2:13])([CH:14]([CH3:15])[CH3:16])[S:17](=...
CN(C)S(=O)(=O)Cl.COc1ccc(CCNC(=O)[C@@H](N)C(C)C)cc1OC
COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)(=O)N(C)C)cc1OC
null
null
O1CCOCC1
Acylation
OtherReaction
03df169542e61bc25f850d05576488c0b54839b94e3082a72ebb3e4f24252841
46615a373e6434dd65776b88d9fcc22218d37124c5265a98f610d7564f54362b
c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[#7:4](-[C;D1;H3:5])-[C;D1;H3:6].[C:7]-[#7:8]-[C:9](=[O;D1;H0:10])-[C@@H;D3;+0:11](-[N;D1;H2:12])-[C:13](-[C;D1;H3:14])-[C;D1;H3:15]>>[C:7]-[#7:8]-[C:9](=[O;D1;H0:10])-[C@;H0;D4;+0:11](-[N;D1;H2:12])(-[C:13](-[C;D1;H3:14])-[C;D1;H3:15])-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H...
null
[]
null
null
null
null
7.2 g of (S)-2-amino-3-methyl-butyric acid N-[2-(3,4-dimethoxyphenyl)-ethyl]-amide and 4 ml of triethylamine are initially introduced in 120 ml of 1,4-dioxane at room temperature, while stirring. 2.8 ml of N,N-dimethylsulfamoyl chloride are added dropwise in the course of 5 minutes. The reaction mixture is then stirred...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1
HCl
O1CCOCC1
null
null
CN(C)S(=O)(=O)Cl.COc1ccc(CCNC(=O)[C@@H](N)C(C)C)cc1OC>O1CCOCC1>COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)(=O)N(C)C)cc1OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-4b5f4cb68ad14383914fad9f4aa70cd0
COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)C(C)C)cc1OC.[O]=[Mn](=[O])(=[O])[O-]>>COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)(=O)C(C)C)cc1OC
[Mn](=O)(=O)(=O)[O-].[K+].COC=1C=C(C=CC1OC)CCNC([C@](C(C)C)(S(=O)C(C)C)N)=O.[Mn](=O)(=O)(=O)[O-]>>COC=1C=C(C=CC1OC)CCNC([C@](C(C)C)(S(=O)(=O)C(C)C)N)=O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][NH:9][C:10](=[O:11])[C@:12]([NH2:13])([CH:14]([CH3:15])[CH3:16])[S:17](=[O:19])[CH:20]([CH3:21])[CH3:22])[cH:23][c:24]1[O:25][CH3:26].[O]=[Mn](=[O])([O-])=[O:18]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][NH:9][C:10](=[O:11])[C@:12]([NH2:13])([CH:14]([CH3:15])...
COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)C(C)C)cc1OC.[O]=[Mn](=[O])(=[O])[O-]
COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)(=O)C(C)C)cc1OC
null
null
CC(=O)C
Oxidation
OtherReaction
4094c25cd21292bb2390398fbe546de8c52271a05feb5a2820ad8177c82110cf
0aef586d3f180a46df69203cc9de96c5ad7ea89db37e5615426f6677f8f720be
c1ccccc1
[C:1]-[C:2](-[N;D1;H2:3])(-[C:4](=[O;D1;H0:5])-[#7:6]-[C:7])-[S;H0;D3;+0:8](=[O;D1;H0:9])-[C:10](-[C;D1;H3:11])-[C;D1;H3:12].[O-]-[Mn](=[O;H0;D1;+0:13])(=[O])=[O]>>[C:1]-[C:2](-[N;D1;H2:3])(-[C:4](=[O;D1;H0:5])-[#7:6]-[C:7])-[S;H0;D4;+0:8](=[O;D1;H0:9])(=[O;H0;D1;+0:13])-[C:10](-[C;D1;H3:11])-[C;D1;H3:12]
null
[]
null
null
45
MINUTE
3.7 g of (S)-2-(isopropylsulfinyl)-amino-3-methyl-butyric acid N-[2-(3,4-dimethoxyphenyl)-ethyl]-amide (Example 3.90) are dissolved in 50 ml of acetone at room temperature. An acetone solution saturated with potassium permanganate is added dropwise to this stirred solution until the reaction mixture retains the violet ...
10.6084/m9.figshare.5104873.v1
null
Sulfoxide
Sulfone
null
null
c1ccccc1
Other
CC(=O)C
null
0.75
COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)C(C)C)cc1OC.[O]=[Mn](=[O])(=[O])[O-]>CC(=O)C>COc1ccc(CCNC(=O)[C@](N)(C(C)C)S(=O)(=O)C(C)C)cc1OC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-f69d3edd52d44422a14f922f370dc48b
Cc1ccc(S(=O)(=O)Cl)cc1.Clc1ccccc1>>Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1
ClC1=CC=CC=C1.[Cl-].[Al+3].[Cl-].[Cl-].C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>CC1=CC=C(C=C1)S(=O)(=O)C2=CC=C(C=C2)Cl
Cl[S:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:17][cH:16]1)(=[O:7])=[O:8].[cH:9]1[cH:10][cH:11][c:12]([Cl:13])[cH:14][cH:15]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[c:9]2[cH:10][cH:11][c:12]([Cl:13])[cH:14][cH:15]2)[cH:16][cH:17]1
Cc1ccc(S(=O)(=O)Cl)cc1.Clc1ccccc1
Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1
null
null
O
Functional Group Interconversion
OtherReaction
36deba09936956b4316cc53d96fe21a3482dda4886181801fc9170bba0f4e08d
fcd366d2a12b9f2b1304281b4b55e60873460be0844fd3f482f05b099eb21cf7
O=S(=O)(c1ccccc1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[c:7]:[c:8]:[cH;D2;+0:9]:[c:10]:[c:11]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[c:4](:[c:5]):[c:6])-[c;H0;D3;+0:9](:[c:8]:[c:7]):[c:10]:[c:11]
null
[]
55
CELSIUS
3
HOUR
To 150 ml of chlorobenzene, 100.1 g (0.75 mol) of aluminum chloride was added, and further 143 g (0.75 mol) of p-toluenesulfonyl chloride was added dropwise over 1 hour. After stirred for 3 hours at 55° C., the reaction mixture was poured into 1.5 liter of water, and then the obtained crystal was filtered off and washe...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Sulfonyl halide
Tosylate
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HCl
O
55
3
Cc1ccc(S(=O)(=O)Cl)cc1.Clc1ccccc1>O>Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ceb80269f1a342758c971e5e753be1b3
Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1.O=C(O)CS>>Cc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1
CC(C)O.CC1=CC=C(C=C1)S(=O)(=O)C2=CC=C(C=C2)Cl.C(CS)(=O)O.[OH-].[K+]>>CC1=CC=C(C=C1)S(=O)(=O)C1=CC=C(C=C1)CC(=S)O
Cl[c:12]1[cH:11][cH:10][c:9]([S:6]([c:5]2[cH:4][cH:3][c:2]([CH3:1])[cH:20][cH:19]2)(=[O:7])=[O:8])[cH:18][cH:17]1.O=[C:13]([CH2:14][SH:16])[OH:15]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7])(=[O:8])[c:9]2[cH:10][cH:11][c:12]([CH2:13][C:14]([OH:15])=[S:16])[cH:17][cH:18]2)[cH:19][cH:20]1
Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1.O=C(O)CS
Cc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1
null
null
CN(C=O)C.O
Acylation
OtherReaction
980d98ef4cff4e80fbd917f0526f30a1edfd5a34853250effb1682e610753519
f99f3b1b8bff52575f3754c7ceba936ca4a0377e8b7a16a1536128e4240695d4
O=S(=O)(c1ccccc1)c1ccccc1
Cl-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].O=[C;H0;D3;+0:6](-[OH;D1;+0:7])-[CH2;D2;+0:8]-[SH;D1;+0:9]>>[OH;D1;+0:7]-[C;H0;D3;+0:8](=[S;H0;D1;+0:9])-[CH2;D2;+0:6]-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
120
CELSIUS
6
HOUR
In 250 ml of N,N-dimethylformamide, 140 g of 4-methyl-4'-chlorodiphenylsulfone was dissolved, and further 77 g of thioglycolic acid and 71 g of 85% potassium hydroxide pellet were added and stirred for 6 hours at 120° C. The reaction mixture was poured into 2-propanol and filtered off to obtain a precipitate. After the...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carboxylic acid.Aliphatic thiol
Thiocarbonyl
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
HCl
CN(C=O)C.O
120
6
Cc1ccc(S(=O)(=O)c2ccc(Cl)cc2)cc1.O=C(O)CS>CN(C=O)C.O>Cc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-18b5af8851614af6b29619286f6beb4b
CCc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1.Cc1ccc(S(=O)(=O)c2ccc(S(=O)(=O)CC(=O)O)cc2)cc1>>CCc1ccc(S(=O)(=O)c2ccc(S(=O)(=O)CC(=O)O)cc2)cc1
CC1=CC=C(C=C1)S(=O)(=O)C1=CC=C(C=C1)S(=O)(=O)CC(=O)O.C(C)C1=CC=C(C=C1)S(=O)(=O)C1=CC=C(C=C1)CC(=S)O>>C(C)C1=CC=C(C=C1)S(=O)(=O)C1=CC=C(C=C1)S(=O)(=O)CC(=O)O
O=S(=O)(c1ccc(CC(O)=S)cc1)c1ccc(C[CH3:1])cc1.[CH3:2][c:3]1[cH:4][cH:5][c:6]([S:7](=[O:8])(=[O:9])[c:10]2[cH:11][cH:12][c:13]([S:14](=[O:15])(=[O:16])[CH2:17][C:18](=[O:19])[OH:20])[cH:21][cH:22]2)[cH:23][cH:24]1>>[CH3:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([S:7](=[O:8])(=[O:9])[c:10]2[cH:11][cH:12][c:13]([S:14](=[O:15])(=[O:...
CCc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1.Cc1ccc(S(=O)(=O)c2ccc(S(=O)(=O)CC(=O)O)cc2)cc1
CCc1ccc(S(=O)(=O)c2ccc(S(=O)(=O)CC(=O)O)cc2)cc1
null
null
null
C-C Coupling
C-methylation
0d792d43f0e84cdc445469eaab43b42dbd3bb565785bce19074c0f35bf28b708
72ed4a4d50b24ee609b5dd3617a985d9e1247237aa6a989345a62e0ac155b36d
O=S(=O)(c1ccccc1)c1ccccc1
O-C(=S)-C-c1:c:c:c(-S(=O)(=O)-c2:c:c:c(-C-[CH3;D1;+0:1]):c:c:2):c:c:1.[CH3;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[CH3;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
null
null
null
null
The intended 4-(4-ethylphenylsulfonyl)phenylsulfonyl acetic acid was prepared in the same manner as in the synthesis of 4-(4-methylphenylsulfonyl)phenylsulfonyl acetic acid of Example 6 except that 104 g of 4-(4-ethylphenylsulfonyl)phenylthio acetic acid was used in place of 100 g of 4-(4-methylphenylsulfonyl)phenylthi...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Thiocarbonyl.Sulfone
null
c1ccccc1.c1ccccc1
null
c1ccccc1.c1ccccc1
TsOH
null
null
null
CCc1ccc(S(=O)(=O)c2ccc(CC(O)=S)cc2)cc1.Cc1ccc(S(=O)(=O)c2ccc(S(=O)(=O)CC(=O)O)cc2)cc1>>CCc1ccc(S(=O)(=O)c2ccc(S(=O)(=O)CC(=O)O)cc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8a215651ccfd41dd9aa2a1416e37b1fc
COc1ccc(C(=O)c2ccc(OC)cc2OC)c(OC)c1>>O=C(c1ccc(O)cc1O)c1ccc(O)cc1O
[Al+3].[Cl-].[Cl-].[Cl-].CN(C=O)C.COC1=C(C(=O)C2=C(C=C(C=C2)OC)OC)C=CC(=C1)OC>>OC1=C(C(=O)C2=C(C=C(C=C2)O)O)C=CC(=C1)O
C[O:7][c:6]1[cH:5][cH:4][c:3]([C:2](=[O:1])[c:11]2[cH:12][cH:13][c:14]([O:15]C)[cH:16][c:17]2[O:18]C)[c:9]([O:10]C)[cH:8]1>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][c:6]([OH:7])[cH:8][c:9]1[OH:10])[c:11]1[cH:12][cH:13][c:14]([OH:15])[cH:16][c:17]1[OH:18]
COc1ccc(C(=O)c2ccc(OC)cc2OC)c(OC)c1
O=C(c1ccc(O)cc1O)c1ccc(O)cc1O
null
null
O
Deprotection
OtherReaction
c9880ca160f0c4ae2189b61831917f8d0a43b3234e3cf24dfacfce49c06cf551
5bfe12e4c5805fe4d4a54cd53f600057b4fffbdf3214f3b83139c3362aecb6bc
O=C(c1ccccc1)c1ccccc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]-[C:4](=[O;D1;H0:5])-[c:6]:[c:7](-[O;H0;D2;+0:8]-C):[c:9]:[c:10](-[O;H0;D2;+0:11]-C):[c:12]):[c:13]:[c:14](-[O;H0;D2;+0:15]-C):[c:16]>>[O;D1;H0:5]=[C:4](-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]:[c:10](-[OH;D1;+0:11]):[c:12])-[c:3]:[c:2](-[OH;D1;+0:1]):[c:13]:[c:14](-[OH;D1;+0:15]):[c:16]
null
[]
30
CELSIUS
4.5
HOUR
440 g (3.30 mol) of AlCl3 were stirred into 120 g (1.64 mol) of dimethylformamide in such a way that the temperature remained below 160° C. After cooling to 30° C., 60.5 g (0.20 mol) of 2,2',4,4'-tetramethoxybenzophenone were introduced into the mixture, which was easily stirrable. The mixture was stirred at about 50°-...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Ether
Aromatic alcohol.Aromatic alcohol.Aromatic alcohol.Aromatic alcohol
null
null
c1ccccc1.c1ccccc1
Other
O
30
4.5
COc1ccc(C(=O)c2ccc(OC)cc2OC)c(OC)c1>O>O=C(c1ccc(O)cc1O)c1ccc(O)cc1O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-3dda345d3c8b43eca91644036bf8ff3e
COc1ccc(C(=O)c2ccc(OC)cc2O)c(O)c1>>O=C(c1ccc(O)cc1O)c1ccc(O)cc1O
OC1=C(C(=O)C2=C(C=C(C=C2)OC)O)C=CC(=C1)OC.[Al+3].[Cl-].[Cl-].[Cl-].CN(C=O)C>>OC1=C(C(=O)C2=C(C=C(C=C2)O)O)C=CC(=C1)O
C[O:7][c:6]1[cH:5][cH:4][c:3]([C:2](=[O:1])[c:11]2[cH:12][cH:13][c:14]([O:15]C)[cH:16][c:17]2[OH:18])[c:9]([OH:10])[cH:8]1>>[O:1]=[C:2]([c:3]1[cH:4][cH:5][c:6]([OH:7])[cH:8][c:9]1[OH:10])[c:11]1[cH:12][cH:13][c:14]([OH:15])[cH:16][c:17]1[OH:18]
COc1ccc(C(=O)c2ccc(OC)cc2O)c(O)c1
O=C(c1ccc(O)cc1O)c1ccc(O)cc1O
null
null
null
Deprotection
OtherReaction
a0f05885bbc65ae2846cad0ac34029941211b2ef3a426958b0c8aa83bb16fe86
9df751cd682ad9d54ed75d7313aaead6a019c5d37ede15c4672866d319b900ff
O=C(c1ccccc1)c1ccccc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4].C-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]
null
[]
null
null
null
null
82.2 g (0.30 mol) of 2,2'-dihydroxy-4,4'-dimethoxybenzophenone were reacted with 600 g of AlCl3 (4.50 mol) and 180 g (2.47 mol) of DMF (dimethylformamide) as in Example 2, and the product was worked up as described. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ether.Ether
Aromatic alcohol.Aromatic alcohol
null
null
c1ccccc1.c1ccccc1
Other
null
null
null
COc1ccc(C(=O)c2ccc(OC)cc2O)c(O)c1>>O=C(c1ccc(O)cc1O)c1ccc(O)cc1O
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-86e31c9534414a65b91ab486505f6497
[OH-].c1ccc([P+]2(c3ccccc3)Cc3ccc4ccccc4c3-c3c(ccc4ccccc34)C2)cc1>>Cc1ccc2ccccc2c1-c1c(CP(=O)(c2ccccc2)c2ccccc2)ccc2ccccc12
[Br-].C1(=CC=CC=C1)[P+]1(CC2=C(C3=C(C1)C=CC1=CC=CC=C13)C=1C=CC=CC1C=C2)C2=CC=CC=C2.[OH-].[Na+]>>C1(=CC=CC=C1)P(=O)(C1=CC=CC=C1)CC1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)C
[OH-:16].[CH2:1]1[c:2]2[cH:3][cH:4][c:5]3[cH:6][cH:7][cH:8][cH:9][c:10]3[c:11]2-[c:12]2[c:13]([cH:29][cH:30][c:31]3[cH:32][cH:33][cH:34][cH:35][c:36]23)[CH2:14][P+:15]1([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)[c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][cH:8][cH:9][c:10]2...
[OH-].c1ccc([P+]2(c3ccccc3)Cc3ccc4ccccc4c3-c3c(ccc4ccccc34)C2)cc1
Cc1ccc2ccccc2c1-c1c(CP(=O)(c2ccccc2)c2ccccc2)ccc2ccccc12
null
null
C(C)O
Miscellaneous
OtherReaction
5bbd0389cac30f4d822c38d363c23ec25049966d8c909010dd2b41dcd38128d0
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
O=P(Cc1ccc2ccccc2c1-c1cccc2ccccc12)(c1ccccc1)c1ccccc1
[OH-;D0:1].[c:2]:[c:3](:[c:4])-[CH2;D2;+0:5]-[P+;H0;D4:6](-[c:7](:[c:8]):[c:9])(-[c:10](:[c:11]):[c:12])-[C:13]-[c:14]>>[CH3;D1;+0:5]-[c:3](:[c:2]):[c:4].[O;H0;D1;+0:1]=[P;H0;D4;+0:6](-[C:13]-[c:14])(-[c:7](:[c:8]):[c:9])-[c:10](:[c:11]):[c:12]
null
[]
null
null
4
HOUR
4 g (7.3 mmol) of 4,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide are suspended in a mixture of 80 ml of 2N sodium hydroxide solution and 30 ml of ethanol and heated to boiling for 4 hours. The reaction solution is subsequently evaporated to dryness at 12 torr/40° C. The residue is taken up i...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c(c1)ccc1c2c2c(ccc3ccccc32)C[P+]C1
null
c1ccc2ccccc2c1.c1ccccc1.c1ccccc1.c1ccc2ccccc2c1
null
C(C)O
null
4
[OH-].c1ccc([P+]2(c3ccccc3)Cc3ccc4ccccc4c3-c3c(ccc4ccccc34)C2)cc1>C(C)O>Cc1ccc2ccccc2c1-c1c(CP(=O)(c2ccccc2)c2ccccc2)ccc2ccccc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-baa38a8e99a645bba8da7e83b29c024a
c1ccc([P+]2(c3ccccc3)Cc3ccc4ccccc4c3-c3c(ccc4ccccc34)C2)cc1>>Cc1ccc2ccccc2c1-c1c(CP(c2ccccc2)c2ccccc2)ccc2ccccc12
[Br-].C1(=CC=CC=C1)[P+]1(CC2=C(C3=C(C1)C=CC1=CC=CC=C13)C=1C=CC=CC1C=C2)C2=CC=CC=C2.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C1(=CC=CC=C1)P(C1=CC=CC=C1)CC1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)C
[CH2:1]1[c:2]2[cH:3][cH:4][c:5]3[cH:6][cH:7][cH:8][cH:9][c:10]3[c:11]2-[c:12]2[c:13]([cH:28][cH:29][c:30]3[cH:31][cH:32][cH:33][cH:34][c:35]23)[CH2:14][P+:15]1([c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)[c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][cH:8][cH:9][c:10]2[c:11]1-[...
c1ccc([P+]2(c3ccccc3)Cc3ccc4ccccc4c3-c3c(ccc4ccccc34)C2)cc1
Cc1ccc2ccccc2c1-c1c(CP(c2ccccc2)c2ccccc2)ccc2ccccc12
null
null
C1(=CC=CC=C1)C
Functional Group Interconversion
OtherReaction
99e36e7f52659b807e758dbd044711de397b08e18d3b7e50a1c0905b20968cc8
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc(P(Cc2ccc3ccccc3c2-c2cccc3ccccc23)c2ccccc2)cc1
[c:1]:[c:2](:[c:3])-[CH2;D2;+0:4]-[P+;H0;D4:5](-[c:6](:[c:7]):[c:8])(-[c:9](:[c:10]):[c:11])-[C:12]-[c:13]>>[CH3;D1;+0:4]-[c:2](:[c:1]):[c:3].[c:13]-[C:12]-[P;H0;D3;+0:5](-[c:6](:[c:7]):[c:8])-[c:9](:[c:10]):[c:11]
null
[]
null
null
5
HOUR
4 g (7.3 mmol) of 4,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide are suspended under a protective gas in 70 ml of absolute toluene. 500 mg (14.3 mmol) of lithium aluminum hydride are added to this suspension and the reaction solution is heated to boiling for 5 hours. Unreacted lithium alumin...
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c(c1)ccc1c2c2c(ccc3ccccc32)C[P+]C1
null
c1ccc2ccccc2c1.c1ccccc1.c1ccccc1.c1ccc2ccccc2c1
null
C1(=CC=CC=C1)C
null
5
c1ccc([P+]2(c3ccccc3)Cc3ccc4ccccc4c3-c3c(ccc4ccccc34)C2)cc1>C1(=CC=CC=C1)C>Cc1ccc2ccccc2c1-c1c(CP(c2ccccc2)c2ccccc2)ccc2ccccc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9002cf0b40e547a59ee61a744aa9df18
c1ccc([P+]2(c3ccccc3)Cc3ccccc3-c3ccccc3C2)cc1>>Cc1ccccc1-c1ccccc1CP(c1ccccc1)c1ccccc1
[Br-].C1(=CC=CC=C1)[P+]1(CC2=C(C3=C(C1)C=CC=C3)C=CC=C2)C2=CC=CC=C2.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C1(=CC=CC=C1)P(C1=CC=CC=C1)CC1=C(C=CC=C1)C1=C(C=CC=C1)C
[CH2:1]1[c:2]2[cH:3][cH:4][cH:5][cH:6][c:7]2-[c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[CH2:14][P+:15]1([c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1)[c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][cH:6][c:7]1-[c:8]1[cH:9][cH:10][cH:11][cH:12][c:13]1[CH2:14][P:15]([c:16]1[cH:17][cH:18][cH:19][c...
c1ccc([P+]2(c3ccccc3)Cc3ccccc3-c3ccccc3C2)cc1
Cc1ccccc1-c1ccccc1CP(c1ccccc1)c1ccccc1
null
null
C1(=CC=CC=C1)C
Functional Group Interconversion
OtherReaction
69605d87899dc0bfea47a101915113dc9389e4ef5e20d0bf01dae30198c0031e
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc(-c2ccccc2CP(c2ccccc2)c2ccccc2)cc1
[c:1]-[C:2]-[P+;H0;D4:3](-[c:4](:[c:5]):[c:6])(-[c:7](:[c:8]):[c:9])-[CH2;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[CH3;D1;+0:10]-[c:11](:[c:12]):[c:13].[c:1]-[C:2]-[P;H0;D3;+0:3](-[c:4](:[c:5]):[c:6])-[c:7](:[c:8]):[c:9]
null
[]
null
null
null
null
4 g (9.0 mmol) of 6,6-diphenyl-6,7-dihydro-5H-dibenzo-[c,e]phosphepinium bromide are suspended in 70 ml of absolute toluene under protective gas and reacted with 680 mg (18 mmol) of lithium aluminum hydride using a method analogous to Example 5. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c(c1)C[P+]Cc1ccccc12
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
null
C1(=CC=CC=C1)C
null
null
c1ccc([P+]2(c3ccccc3)Cc3ccccc3-c3ccccc3C2)cc1>C1(=CC=CC=C1)C>Cc1ccccc1-c1ccccc1CP(c1ccccc1)c1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-9144b195488a484e95660584bc9d7fc6
CCC(C)[P+]1(C(C)CC)Cc2ccc3ccccc3c2-c2c(ccc3ccccc23)C1>>CCC(C)P(Cc1ccc2ccccc2c1-c1c(C)ccc2ccccc12)C(C)CC
[Br-].CC(CC)[P+]1(CC2=C(C3=C(C1)C=CC1=CC=CC=C13)C=1C=CC=CC1C=C2)C(CC)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>CC(CC)P(C(CC)C)CC1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)C
[CH3:1][CH2:2][CH:3]([CH3:4])[P+:5]1([CH:28]([CH3:29])[CH2:30][CH3:31])[CH2:6][c:7]2[cH:8][cH:9][c:10]3[cH:11][cH:12][cH:13][cH:14][c:15]3[c:16]2-[c:17]2[c:18]([cH:20][cH:21][c:22]3[cH:23][cH:24][cH:25][cH:26][c:27]23)[CH2:19]1>>[CH3:1][CH2:2][CH:3]([CH3:4])[P:5]([CH2:6][c:7]1[cH:8][cH:9][c:10]2[cH:11][cH:12][cH:13][cH...
CCC(C)[P+]1(C(C)CC)Cc2ccc3ccccc3c2-c2c(ccc3ccccc23)C1
CCC(C)P(Cc1ccc2ccccc2c1-c1c(C)ccc2ccccc12)C(C)CC
null
null
C=1(C(=CC=CC1)C)C
Functional Group Interconversion
OtherReaction
99e36e7f52659b807e758dbd044711de397b08e18d3b7e50a1c0905b20968cc8
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc2c(-c3cccc4ccccc34)cccc2c1
[C:1]-[C:2](-[C;D1;H3:3])-[P+;H0;D4:4](-[C:5](-[C:6])-[C;D1;H3:7])(-[C:8]-[c:9])-[CH2;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[CH3;D1;+0:10]-[c:11](:[c:12]):[c:13].[C:1]-[C:2](-[C;D1;H3:3])-[P;H0;D3;+0:4](-[C:8]-[c:9])-[C:5](-[C:6])-[C;D1;H3:7]
null
[]
null
null
null
null
4 g (7.9 mmol) of 4,4-di(1'-methylpropyl)-4,5-dihydro-3H-dinaphtho[2,1-c:1',2'-e]phosphepinium bromide are suspended in 70 ml of absolute xylene and reacted with 400 mg (10.5 mmol) of lithium aluminum hydride using a method analogous to Example 5. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c(c1)ccc1c2c2c(ccc3ccccc32)C[P+]C1
null
c1ccc2ccccc2c1.c1ccc2ccccc2c1
null
C=1(C(=CC=CC1)C)C
null
null
CCC(C)[P+]1(C(C)CC)Cc2ccc3ccccc3c2-c2c(ccc3ccccc23)C1>C=1(C(=CC=CC1)C)C>CCC(C)P(Cc1ccc2ccccc2c1-c1c(C)ccc2ccccc12)C(C)CC
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-7819582fed694c3f99e1f2746fab150a
CC(C)[P+]1(C(C)C)Cc2ccc3ccccc3c2-c2c(ccc3ccccc23)C1>>Cc1ccc2ccccc2c1-c1c(CP(C(C)C)C(C)C)ccc2ccccc12
[Br-].C(C)(C)[P+]1(CC2=C(C3=C(C1)C=CC1=CC=CC=C13)C=1C=CC=CC1C=C2)C(C)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>C(C)(C)P(C(C)C)CC1=C(C2=CC=CC=C2C=C1)C1=C(C=CC2=CC=CC=C12)C
[CH2:1]1[c:2]2[cH:3][cH:4][c:5]3[cH:6][cH:7][cH:8][cH:9][c:10]3[c:11]2-[c:12]2[c:13]([cH:22][cH:23][c:24]3[cH:25][cH:26][cH:27][cH:28][c:29]23)[CH2:14][P+:15]1([CH:16]([CH3:17])[CH3:18])[CH:19]([CH3:20])[CH3:21]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[cH:6][cH:7][cH:8][cH:9][c:10]2[c:11]1-[c:12]1[c:13]([CH2:14][P:15]([CH:16](...
CC(C)[P+]1(C(C)C)Cc2ccc3ccccc3c2-c2c(ccc3ccccc23)C1
Cc1ccc2ccccc2c1-c1c(CP(C(C)C)C(C)C)ccc2ccccc12
null
null
C1(=CC=CC=C1)C
Functional Group Interconversion
OtherReaction
99e36e7f52659b807e758dbd044711de397b08e18d3b7e50a1c0905b20968cc8
f1bbf9aa3c82f5e49be9f6d53533b6bb152f359232b6d32090c168949766aa71
c1ccc2c(-c3cccc4ccccc34)cccc2c1
[C;D1;H3:1]-[C:2](-[C;D1;H3:3])-[P+;H0;D4:4](-[C:5](-[C;D1;H3:6])-[C;D1;H3:7])(-[C:8]-[c:9])-[CH2;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[C;D1;H3:1]-[C:2](-[C;D1;H3:3])-[P;H0;D3;+0:4](-[C:8]-[c:9])-[C:5](-[C;D1;H3:6])-[C;D1;H3:7].[CH3;D1;+0:10]-[c:11](:[c:12]):[c:13]
null
[]
null
null
null
null
4 g (8.4 mmol) of 4,4-diisopropyl-4,5-dihydro-3H-dinaphtho[2,1-c:1',2'-e]phosphepinium bromide are suspended in 70 ml of absolute toluene under protective gas and reacted with 400 mg (10.5 mmol) of lithium aluminum hydride using a method analogous to Example 5. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
null
null
c1ccc2c(c1)ccc1c2c2c(ccc3ccccc32)C[P+]C1
null
c1ccc2ccccc2c1.c1ccc2ccccc2c1
null
C1(=CC=CC=C1)C
null
null
CC(C)[P+]1(C(C)C)Cc2ccc3ccccc3c2-c2c(ccc3ccccc23)C1>C1(=CC=CC=C1)C>Cc1ccc2ccccc2c1-c1c(CP(C(C)C)C(C)C)ccc2ccccc12
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-c24b8279498c4f1780da6e8b6f498cbc
CCCCCCCC=O.O=Cc1ccccc1>>CCCCCCC(C=O)=Cc1ccccc1.CCCCCCCC=O.O=Cc1ccccc1
C(CCCCCCC)=O.C(C1=CC=CC=C1)=O>>C(C1=CC=CC=C1)=O.C(CCCCCCC)=O.C(CCCCC)C(C=O)=CC1=CC=CC=C1
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[O:9].[cH:10]1[cH:31][cH:30][cH:29][c:28]([CH:27]=[O:26])[cH:33]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([CH:8]=[O:9])=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1.[CH3:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH:24]=[O:25].[O:26]=[CH:27...
CCCCCCCC=O.O=Cc1ccccc1
CCCCCCC(C=O)=Cc1ccccc1.CCCCCCCC=O.O=Cc1ccccc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
0372dbf87c8b3baa6111ae193e012612acfceb9695609df4651d1b12bc52db67
f2d6b3b078203bee78dabcac04571761da415ea369d366eb759c2728ef152f21
c1ccccc1.c1ccccc1
[C:1]-[C:2]-[CH2;D2;+0:3]-[C:4]=[O;D1;H0:5].[O;D1;H0:6]=[C:7]-[c:8]1:[c:9]:[c:10]:[cH;D2;+0:11]:[cH;D2;+0:12]:[cH;D2;+0:13]:1>>[C:1]-[C:2]-[C;H0;D3;+0:3](-[C:4]=[O;D1;H0:5])=[CH;D2;+0:12]-[c:14](:[c:15]):[c:16].[O;D1;H0:6]=[C:7]-[c:8]1:[c:9]:[c:10]:[cH;D2;+0:11]:[c:17]:[cH;D2;+0:13]:1
null
[]
null
null
null
null
The conversion of the benzaldehyde (bald) amounted to 65.6% and the degree of conversion of octanal to 100%. The selectivities of benzaldehyde and octanal to give α-hexylcinnamaldehyde (α-hex) were 94.9% and 96.2%, respectively, while the selectivity of octanal to give α-hexyldecenal (α-HD) was 1.0%. Conditions: See re...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Aldehyde.Aldehyde
c1ccccc1
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1
Other
null
null
null
CCCCCCCC=O.O=Cc1ccccc1>>CCCCCCC(C=O)=Cc1ccccc1.CCCCCCCC=O.O=Cc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-d3c682656e894ba7964c3b5aa97e319e
CCCCCCCC=O.O=Cc1ccccc1>>CCCCCCC(C=O)=Cc1ccccc1
C(CCCCCCC)=O.C(C1=CC=CC=C1)=O.N1CCCC1.C1(=CC=CC=C1)NC1=CC=CC=C1.C(C)(=O)O.[OH-].[Na+].C(C)(=O)O.C(CCCCCCC)=O>>C(CCCCC)C(C=O)=CC1=CC=CC=C1
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[O:9].O=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([CH:8]=[O:9])=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
CCCCCCCC=O.O=Cc1ccccc1
CCCCCCC(C=O)=Cc1ccccc1
null
null
null
C-C Coupling
OtherReaction
154f038b7f5648ae5349abff8a924c982177f620bdfb6a2f53d7ca0fce37c68d
3174a51604157c488f07402e36f994f716989b8fc10687ee243713b4cfbdb11a
c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[CH2;D2;+0:7]-[C:8]=[O;D1;H0:9]>>[C:5]-[C:6]-[C;H0;D3;+0:7](-[C:8]=[O;D1;H0:9])=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
85
CELSIUS
180
MINUTE
The reaction was carried out in a 2.5 litre double-walled glass reactor provided with a cooler, turbine stirrer (6 blades), thermocouple and a submerged metering tube. A mixture of 1065 grams of benzaldehyde (10.0 mol), 48.8 grams of pyrrolidine (0.679 mol) and 1.8 grams of diphenylamine was heated to 85° C. Over a per...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Aldehyde
Aldehyde
null
null
c1ccccc1
HO-
null
85
3
CCCCCCCC=O.O=Cc1ccccc1>>CCCCCCC(C=O)=Cc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-8d50ad566a2f43caa35ed18dd7496bf1
CCCCCCCC=O.O=Cc1ccccc1>>CCCCCCC(C=O)=Cc1ccccc1
C(C1=CC=CC=C1)=O.C(CCCCCCC)=O>>C(CCCCC)C(C=O)=CC1=CC=CC=C1
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[O:9].O=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([CH:8]=[O:9])=[CH:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1
CCCCCCCC=O.O=Cc1ccccc1
CCCCCCC(C=O)=Cc1ccccc1
null
null
null
C-C Coupling
OtherReaction
154f038b7f5648ae5349abff8a924c982177f620bdfb6a2f53d7ca0fce37c68d
3174a51604157c488f07402e36f994f716989b8fc10687ee243713b4cfbdb11a
c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6]-[CH2;D2;+0:7]-[C:8]=[O;D1;H0:9]>>[C:5]-[C:6]-[C;H0;D3;+0:7](-[C:8]=[O;D1;H0:9])=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
The method of claim 1 or 2, wherein α-hexylcinnamaldehyde is prepared via aldol condensation of benzaldehyde and n-octanal. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Aldehyde
Aldehyde
null
null
c1ccccc1
HO-
null
null
null
CCCCCCCC=O.O=Cc1ccccc1>>CCCCCCC(C=O)=Cc1ccccc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-ef5596a4da4243beba3c5680c17f513e
ClCc1ccccc1.O>>OCc1ccccc1.c1ccc(COCc2ccccc2)cc1
C(C1=CC=CC=C1)Cl.O>>C(C1=CC=CC=C1)O.C(C1=CC=CC=C1)OCC1=CC=CC=C1
Cl[CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1.[OH2:1]>>[OH:1][CH2:2][c:3]1[cH:4][cH:5][cH:6][cH:7][cH:8]1.[cH:9]1[cH:10][cH:11][c:12]([CH2:13][O:14][CH2:15][c:16]2[cH:17][cH:18][cH:19][cH:20][cH:21]2)[cH:22][cH:23]1
ClCc1ccccc1.O
OCc1ccccc1.c1ccc(COCc2ccccc2)cc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
b3d5a94c37a1c91f1c785fd36b5598c0ee81262b64aead6380d2022741e043ad
e60a1287d01749b8d52e42fb3423e3f2559430d2de6ab05369b4de69515bcf91
c1ccc(COCc2ccccc2)cc1.c1ccccc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[OH2;D0;+0:5]>>[OH;D1;+0:5]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
5.4
[{"value": 5.4, "product": "C(C1=CC=CC=C1)OCC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
126.5 g (1 mol) of benzyl chloride and 180 g (10 mol) of water were rapidly heated to reflux in a flask with baffles and propeller stirrer with vigorous stirring (250 rpm) under nitrogen. After 240 min reaction time, the mixture was rapidly cooled, the organic phase was separated off after addition of toluene, and anal...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Ether.Primary alcohol
null
c1ccccc1.c1ccccc1
c1ccccc1.c1ccccc1.c1ccccc1
null
null
null
null
ClCc1ccccc1.O>>OCc1ccccc1.c1ccc(COCc2ccccc2)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-3ced4cee9a3c4c979b4e3a0eb0a11cbb
COc1ccccc1N.O=S(=O)(Cl)c1cccnc1>>COc1ccccc1NS(=O)(=O)c1cccnc1
C([O-])([O-])=O.[Na+].[Na+].N1=CC=CC=C1.COC=1C(=CC=CC1)N.Cl.N1=CC(=CC=C1)S(=O)(=O)Cl>>COC1=C(C=CC=C1)NS(=O)(=O)C=1C=NC=CC1
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[NH2:9].Cl[S:10](=[O:11])(=[O:12])[c:13]1[cH:14][cH:15][cH:16][n:17][cH:18]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[NH:9][S:10](=[O:11])(=[O:12])[c:13]1[cH:14][cH:15][cH:16][n:17][cH:18]1
COc1ccccc1N.O=S(=O)(Cl)c1cccnc1
COc1ccccc1NS(=O)(=O)c1cccnc1
null
null
C1(=CC=CC=C1)C.O
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=S(=O)(Nc1ccccc1)c1cccnc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6]:[#7;a:7]:[c:8].[NH2;D1;+0:9]-[c:10](:[c:11]):[c:12]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:9]-[c:10](:[c:11]):[c:12])-[c:4](:[c:5]):[c:6]:[#7;a:7]:[c:8]
83.5
[{"value": 83.5, "product": "COC1=C(C=CC=C1)NS(=O)(=O)C=1C=NC=CC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 83.5, "product": "COC1=C(C=CC=C1)NS(=O)(=O)C=1C=NC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
1.5
HOUR
o-Anisidine (377 mg, 3.0 mmol) was dissolved in toluene (10 ml) to which were subsequently added pyridine (0.48 ml, 6.0 mmol) and 3-pyridinesulfonylchloride hydrochloride (642 mg, 3.0 mmol) at room temperature. After 1.5 hours of stirring at 100° C., the resulting reaction solution was mixed with water (20 ml), adjuste...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccncc1
HCl
C1(=CC=CC=C1)C.O
100
1.5
COc1ccccc1N.O=S(=O)(Cl)c1cccnc1>C1(=CC=CC=C1)C.O>COc1ccccc1NS(=O)(=O)c1cccnc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-04e2e891f8e24233803e97b3a1a02cf4
COc1ccccc1N.Cc1ccc(S(=O)(=O)Cl)cc1>>COc1ccccc1NS(=O)(=O)c1ccc(C)cc1
O.N1=CC=CC=C1.COC=1C(=CC=CC1)N.C1(=CC=C(C=C1)S(=O)(=O)Cl)C>>COC1=C(C=CC=C1)NS(=O)(=O)C1=CC=C(C=C1)C
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[NH2:9].Cl[S:10](=[O:11])(=[O:12])[c:13]1[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[NH:9][S:10](=[O:11])(=[O:12])[c:13]1[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]1
COc1ccccc1N.Cc1ccc(S(=O)(=O)Cl)cc1
COc1ccccc1NS(=O)(=O)c1ccc(C)cc1
null
CN(C1=CC=NC=C1)C
C1(=CC=CC=C1)C
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
84f0a2c480e4021adb28613388cdf35ca03a8bd65bbdad356e160a1b94684976
2988afdf4a13d931f021994343ac8648c6e63ca3a4c0ba598a4b99bbffc001c8
O=S(=O)(Nc1ccccc1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10])-[c:4](:[c:5]):[c:6]
62
[{"value": 62.0, "product": "COC1=C(C=CC=C1)NS(=O)(=O)C1=CC=C(C=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 62.0, "product": "COC1=C(C=CC=C1)NS(=O)(=O)C1=CC=C(C=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2.5
HOUR
o-Anisidine (2.34 ml, 20 mmol) was dissolved in toluene (60 ml) to which were subsequently added, with cooling in an ice bath, pyridine (4.58 ml, 60 mmol), p-toluenesulfonyl chloride (3.89 g, 20 mmol) and a catalytically effective amount of 4-dimethylaminopyridine. After 2.5 hours of stirring at room temperature, the r...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccccc1
HCl
CN(C1=CC=NC=C1)C.C1(=CC=CC=C1)C
null
2.5
COc1ccccc1N.Cc1ccc(S(=O)(=O)Cl)cc1>CN(C1=CC=NC=C1)C.C1(=CC=CC=C1)C>COc1ccccc1NS(=O)(=O)c1ccc(C)cc1
ord_dataset-018fd0e1351f4fd09b20fcddd97b4c7a
ord-80f67fcb3ee14ef2b196db2ad72d47b4
COc1ccc(S(=O)(=O)Cl)cc1.COc1ccccc1N>>COc1ccc(S(=O)(=O)Nc2ccccc2OC)cc1
COC=1C(=CC=CC1)N.COC1=CC=C(C=C1)S(=O)(=O)Cl>>COC1=CC=C(C=C1)S(=O)(=O)NC1=C(C=CC=C1)OC
Cl[S:7]([c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:20][cH:19]1)(=[O:8])=[O:9].[NH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][c:16]1[O:17][CH3:18]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([S:7](=[O:8])(=[O:9])[NH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]2[O:17][CH3:18])[cH:19][cH:20]1
COc1ccc(S(=O)(=O)Cl)cc1.COc1ccccc1N
COc1ccc(S(=O)(=O)Nc2ccccc2OC)cc1
null
null
null
Acylation
Sulfonamide synthesis (Schotten-Baumann) primary amine
4c44ef6d7646f6ef25dd125d2c32c713d8dcae7c603407faa5f0fb810631670e
8fce8115d8a725afa92eb3910ded29d4c852e5133eba78a425054f41f7142603
O=S(=O)(Nc1ccccc1)c1ccccc1
Cl-[S;H0;D4;+0:1](=[O;D1;H0:2])(=[O;D1;H0:3])-[c:4](:[c:5]):[c:6].[NH2;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[O;D1;H0:2]=[S;H0;D4;+0:1](=[O;D1;H0:3])(-[NH;D2;+0:7]-[c:8](:[c:9]):[c:10])-[c:4](:[c:5]):[c:6]
90.1
[{"value": 90.1, "product": "COC1=CC=C(C=C1)S(=O)(=O)NC1=C(C=CC=C1)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.1, "product": "COC1=CC=C(C=C1)S(=O)(=O)NC1=C(C=CC=C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using o-anisidine (1.0 ml, 8.55 mmol) and 4-methoxybenzenesulfonyl chloride (1.78 g, 8.55 mmol), the procedure of Reference Example 2 was repeated to obtain 2.26 g (90.1%) of the title compound in the form of colorless powder. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
c1ccccc1.c1ccccc1
HCl
null
null
null
COc1ccc(S(=O)(=O)Cl)cc1.COc1ccccc1N>>COc1ccc(S(=O)(=O)Nc2ccccc2OC)cc1