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
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14
3.37k
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large_stringlengths
1
581
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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-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0d3522fbdd884f9ea992a9cf980ff044
O=C1CCCNC12CCc1ccccc1C2>>OC1c2ccccc2CCC12CCCCN2
N1C2(C(CCC1)=O)CC1=CC=CC=C1CC2.CO.[BH4-].[Na+]>>N1C2(CCCC1)C(C1=CC=CC=C1CC2)O
[O:1]=[C:12]1[C:11]2([CH2:2][c:3]3[cH:4][cH:5][cH:6][cH:7][c:8]3[CH2:9][CH2:10]2)[NH:16][CH2:15][CH2:14][CH2:13]1>>[OH:1][CH:2]1[c:3]2[cH:4][cH:5][cH:6][cH:7][c:8]2[CH2:9][CH2:10][C:11]12[CH2:12][CH2:13][CH2:14][CH2:15][NH:16]2
O=C1CCCNC12CCc1ccccc1C2
OC1c2ccccc2CCC12CCCCN2
null
null
O
Miscellaneous
OtherReaction
24b2475629273829480e7d8cf68e36a8c1cd83adc110d39c767e13c6335a3909
65c0f1e474134afe581396038c9eec1081d3cf2c66a067b33a419661521d5253
c1ccc2c(c1)CCC1(CCCCN1)C2
[C:1]-[C:2]1(-[#7:3]-[C:4]-[C:5]-[C:6]-[C;H0;D3;+0:7]-1=[O;H0;D1;+0:8])-[CH2;D2;+0:9]-[c:10](:[c:11]):[c:12]>>[C:1]-[C:2]1(-[#7:3]-[C:4]-[C:5]-[C:6]-[CH2;D2;+0:7]-1)-[CH;D3;+0:9](-[OH;D1;+0:8])-[c:10](:[c:11]):[c:12]
null
[]
null
null
30
MINUTE
In 20 ml of methanol was dissolved 0.80 g of 3,4-dihydrospiro[naphthalene-2(1H),2'-piperidin]-one and following addition of 0.15 g of sodium borohydride in small portions, the mixture was stirred for 30 minutes. The reaction mixture was then diluted with water and extracted with methylene chloride. The methylene chlori...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
c1ccc2c(c1)CCC1(CCCCN1)C2
c1ccc2c(c1)CCC1(CCCCN1)C2
c1ccc2c(c1)CCC1(CCCCN1)C2
null
O
null
0.5
O=C1CCCNC12CCc1ccccc1C2>O>OC1c2ccccc2CCC12CCCCN2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-686546873c7d4c56ba5142ce531de9e0
COc1ccc2c(c1)CCC1(CCCCN1)C2=O>>COc1ccc2c(c1)CCC1(CCCCN1)C2
C(C)[SiH](CC)CC.COC=1C=C2CCC3(NCCCC3)C(C2=CC1)=O.Cl>>Cl.COC=1C=C2CCC3(NCCCC3)CC2=CC1
O=[C:17]1[c:6]2[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:8][c:7]2[CH2:9][CH2:10][C:11]12[CH2:12][CH2:13][CH2:14][CH2:15][NH:16]2>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[CH2:9][CH2:10][C:11]1([CH2:12][CH2:13][CH2:14][CH2:15][NH:16]1)[CH2:17]2
COc1ccc2c(c1)CCC1(CCCCN1)C2=O
COc1ccc2c(c1)CCC1(CCCCN1)C2
null
null
O.FC(C(=O)O)(F)F
Reduction
OtherReaction
40edb481f91ef73120b0cb754905dfaf94acd35da35b5213a026564437b26a90
f9ba67182f94acd5fbe41487f8f71e26bccf898b8fc8091ef46f4363de5628d4
c1ccc2c(c1)CCC1(CCCCN1)C2
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4])-[C:5](-[C:6])(-[C:7])-[#7:8]-[C:9]>>[C:6]-[C:5](-[C:7])(-[#7:8]-[C:9])-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
1
HOUR
In 30 ml of trifluoroacetic acid was dissolved 6.57 g of 3,4-dihydro-6-methoxyspiro[naphthalene-2(1H),2'-piperidin]-1-one followed by addition of 8.5 ml of triethylsilane and the mixture was stirred for 1 hour. This reaction mixture was poured portionwise in water. To this was added 1N-hydrochloric acid and the mixture...
10.6084/m9.figshare.5104873.v1
null
Ketone
null
c1ccc2c(c1)CCC1(CCCCN1)C2
c1ccc2c(c1)CCC1(CCCCN1)C2
c1ccc2c(c1)CCC1(CCCCN1)C2
Other
O.FC(C(=O)O)(F)F
null
1
COc1ccc2c(c1)CCC1(CCCCN1)C2=O>O.FC(C(=O)O)(F)F>COc1ccc2c(c1)CCC1(CCCCN1)C2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-92aedeabdb674b35aa10924e69d9fbbd
BrCc1ccccc1.COc1cc2c(cc1OC)CC1(CCCCN1)CC2>>COc1cc2c(cc1OC)CC1(CCCCN1Cc1ccccc1)CC2
Cl.COC=1C=C2CCC3(NCCCC3)CC2=CC1OC.C([O-])([O-])=O.[K+].[K+].C(C1=CC=CC=C1)Br>>COC=1C=C2CCC3(N(CCCC3)CC3=CC=CC=C3)CC2=CC1OC
Br[CH2:18][c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1.[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH3:10])[CH2:11][C:12]1([CH2:13][CH2:14][CH2:15][CH2:16][NH:17]1)[CH2:25][CH2:26]2>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH3:10])[CH2:11][C:12]1([CH2:13][CH2:14][CH2:15][CH2:16][N:17]1[CH2:18][c:...
BrCc1ccccc1.COc1cc2c(cc1OC)CC1(CCCCN1)CC2
COc1cc2c(cc1OC)CC1(CCCCN1Cc1ccccc1)CC2
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
e76537564b204757c56ea9f15d9563556e48d483b30b2e91436650a0999d405b
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(CN2CCCCC23CCc2ccccc2C3)cc1
Br-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6](-[C:7])(-[C:8])-[NH;D2;+0:9]-[C:10]-[C:11]>>[C:5]-[C:6](-[C:7])(-[C:8])-[N;H0;D3;+0:9](-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:10]-[C:11]
null
[]
null
null
null
null
3,4-Dihydro-6,7-dimethoxyspiro[naphthalene-2(1H),2'-piperidine] hydrochloride (10 mg) was treated with potassium carbonate (10 g) and benzyl bromide (4 ml) in DMF (300 ml) at 60° C. for 2 hours. The reaction product was extracted with ethyl acetate-water, washed with water, dried, and concentrated. Purification with si...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
c1ccc2c(c1)CCC1(CCCCN1)C2
c1ccc2c(c1)CCC1(CCCC[NH]1)C2
c1ccc2c(c1)CCC1(CCCC[NH]1)C2.c1ccccc1
HBr
CN(C)C=O
null
null
BrCc1ccccc1.COc1cc2c(cc1OC)CC1(CCCCN1)CC2>CN(C)C=O>COc1cc2c(cc1OC)CC1(CCCCN1Cc1ccccc1)CC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4cc0c6f610bb40f9a1e1e4c513076ae5
COc1ccc2c(c1)CCC1(CCCCN1C(=O)C(F)(F)F)C2.O.O=C(OC(=O)C(F)(F)F)C(F)(F)F.O=[N+]([O-])[O-].[NH4+]>>COc1cc2c(cc1[N+](=O)[O-])CC1(CCCCN1C(=O)C(F)(F)F)CC2.COc1ccc2c(c1[N+](=O)[O-])CCC1(CCCCN1C(=O)C(F)(F)F)C2
FC(C(=O)OC(C(F)(F)F)=O)(F)F.O.FC(C(=O)N1C2(CCCC1)CC1=CC=C(C=C1CC2)OC)(F)F.[N+](=O)([O-])[O-].[NH4+]>>FC(C(=O)N1C2(CCCC1)CC1=CC(=C(C=C1CC2)OC)[N+](=O)[O-])(F)F.FC(C(=O)N1C2(CCCC1)CC1=CC=C(C(=C1CC2)[N+](=O)[O-])OC)(F)F
[CH3:1][O:2][c:3]1[cH:4][c:33]2[c:32]([cH:31][cH:30]1)[CH2:52][C:13]1([N:18]([C:19](=[O:20])[C:21]([F:22])([F:23])[F:24])[CH2:17][CH2:43][CH2:42][CH2:41]1)[CH2:39][CH2:38]2.[OH2:36].F[C:5](F)(F)[C:27](O[C:15]([C:16]([F:49])([F:50])[F:51])=[O:47])=[O:28].[N+:9](=[O:10])([O-:11])[O-:37].[NH4+:45]>>[CH3:1][O:2][c:3]1[cH:4...
COc1ccc2c(c1)CCC1(CCCCN1C(=O)C(F)(F)F)C2.O.O=C(OC(=O)C(F)(F)F)C(F)(F)F.O=[N+]([O-])[O-].[NH4+]
COc1cc2c(cc1[N+](=O)[O-])CC1(CCCCN1C(=O)C(F)(F)F)CC2.COc1ccc2c(c1[N+](=O)[O-])CCC1(CCCCN1C(=O)C(F)(F)F)C2
null
null
C(Cl)(Cl)Cl
Aromatic Heterocycle Formation
OtherReaction
3a13d919ad36cc369c9146e3aee3c8ebfb823918c4bcd743476089bdf57d5fef
2acc14181a82a68dfc7ff499b15e5d6f8c9c09c327ac75439e4d543595b2222f
c1ccc2c(c1)CCC1(CCCCN1)C2.c1ccc2c(c1)CCC1(CCCCN1)C2
F-[C;H0;D4;+0:1](-F)(-F)-[C;H0;D3;+0:2](=[O;H0;D1;+0:3])-O-[C;H0;D3;+0:4](=[O;H0;D1;+0:5])-[C;H0;D4;+0:6](-[F;H0;D1;+0:7])(-[F;H0;D1;+0:8])-[F;H0;D1;+0:9].[C;D1;H3:10]-[#8:11]-[c;H0;D3;+0:12]1:[cH;D2;+0:13]:[c:14]:[c:15]2:[c;H0;D3;+0:16](:[cH;D2;+0:17]:1)-[C:18]-[CH2;D2;+0:19]-[C;H0;D4;+0:20]1(-[CH2;D2;+0:21]-[C:22]-[C...
null
[]
null
null
8
HOUR
6.0 g of 1'-trifluoroacetyl-3,4-dihydro-6-methoxyspiro[naphthalene-2(1H),2'-piperidine] was dissolved in 150 ml of chloroform. After 1.5 g of ammonium nitrate was suspended in this solution, 9 ml of trifluoroacetic anhydride was added, followed by overnight stirring at room temperature. After water was added, the react...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Trifluoro group.Anhydride.Ether.Nitrate
Trifluoro group.Ether.Ether.Nitro group.Nitro group.Tertiary amide
c1ccc2c(c1)CCC1(CCCC[NH]1)C2
c1ccc2c(c1)CCC1(CCCC[NH]1)C2.c1ccc2c(c1)CCC1(CCCC[NH]1)C2
c1ccc2c(c1)CCC1(CCCC[NH]1)C2.c1ccc2c(c1)CCC1(CCCC[NH]1)C2
null
C(Cl)(Cl)Cl
null
8
COc1ccc2c(c1)CCC1(CCCCN1C(=O)C(F)(F)F)C2.O.O=C(OC(=O)C(F)(F)F)C(F)(F)F.O=[N+]([O-])[O-].[NH4+]>C(Cl)(Cl)Cl>COc1cc2c(cc1[N+](=O)[O-])CC1(CCCCN1C(=O)C(F)(F)F)CC2.COc1ccc2c(c1[N+](=O)[O-])CCC1(CCCCN1C(=O)C(F)(F)F)C2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3b6a2edc981a43d985cbda64672bb38c
CCOC(=O)C1(N)CCc2cc(OC)c(OC)cc2C1.CN(CC(=O)O)C(=O)OCc1ccccc1>>CCOC(=O)C1(NC(=O)CN(C)C(=O)OCc2ccccc2)CCc2cc(OC)c(OC)cc2C1
NC1(CC2=CC(=C(C=C2CC1)OC)OC)C(=O)OCC.C(C1=CC=CC=C1)OC(=O)N(C)CC(=O)O.Cl.C(C)N=C=NCCCN(C)C.C(C)N(CC)CC>>C(C1=CC=CC=C1)OC(=O)N(C)CC(=O)NC1(CC2=CC(=C(C=C2CC1)OC)OC)C(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1([NH2:7])[CH2:23][CH2:24][c:25]2[cH:26][c:27]([O:28][CH3:29])[c:30]([O:31][CH3:32])[cH:33][c:34]2[CH2:35]1.O[C:8](=[O:9])[CH2:10][N:11]([CH3:12])[C:13](=[O:14])[O:15][CH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]1([NH:7][C:8](=[O:9])[CH2:...
CCOC(=O)C1(N)CCc2cc(OC)c(OC)cc2C1.CN(CC(=O)O)C(=O)OCc1ccccc1
CCOC(=O)C1(NC(=O)CN(C)C(=O)OCc2ccccc2)CCc2cc(OC)c(OC)cc2C1
null
null
ClCCl
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(CNC(=O)OCc1ccccc1)NC1CCc2ccccc2C1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#7:4]-[C:5]=[O;D1;H0:6].[C:7]-[C:8](-[NH2;D1;+0:9])(-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13])-[C:14]>>[C:7]-[C:8](-[NH;D2;+0:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#7:4]-[C:5]=[O;D1;H0:6])(-[C:10](=[O;D1;H0:11])-[#8:12]-[C:13])-[C:14]
75.7
[{"value": 74.0, "product": "C(C1=CC=CC=C1)OC(=O)N(C)CC(=O)NC1(CC2=CC(=C(C=C2CC1)OC)OC)C(=O)OCC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 75.7, "product": "C(C1=CC=CC=C1)OC(=O)N(C)CC(=O)NC1(CC2=CC(=C(C=C2CC1)OC)OC)C(=O)OCC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
To a solution of ethyl 2-amino-1,2,3,4-tetrahydro-6,7-dimethoxynaphthalene-2-carboxylate (430 mg, 1.5 mmol), N-benzyloxycarbonylsarcosine (357 mg, 1.6 mmol), and 1-ethyl-3-(3'-dimethylaminopropyl)carbodiimide hydrochloride in dichloromethane (5 ml) was added triethylamine (160 mg, 1.6 mmol) under stirring at 0° C. Afte...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2c(c1)CCCC2
HO-
ClCCl
0
null
CCOC(=O)C1(N)CCc2cc(OC)c(OC)cc2C1.CN(CC(=O)O)C(=O)OCc1ccccc1>ClCCl>CCOC(=O)C1(NC(=O)CN(C)C(=O)OCc2ccccc2)CCc2cc(OC)c(OC)cc2C1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9bd1f43edb1547daa2f9d118ae4fcc96
CCOC(=O)C1(NC(=O)CN(C)C(=O)OCc2ccccc2)CCc2cc(OC)c(OC)cc2C1>>COc1cc2c(cc1OC)CC1(CC2)NC(=O)CC(C)C1=O
C(C1=CC=CC=C1)OC(=O)N(C)CC(=O)NC1(CC2=CC(=C(C=C2CC1)OC)OC)C(=O)OCC.C(C)O>>COC=1C=C2CCC3(NC(CC(C3=O)C)=O)CC2=CC1OC
CCO[C:21]([C:12]1([NH:15][C:16](=[O:17])[CH2:18]N(C(=O)OCc2ccccc2)[CH3:20])[CH2:11][c:6]2[c:5]([cH:4][c:3]([O:2][CH3:1])[c:8]([O:9][CH3:10])[cH:7]2)[CH2:14][CH2:13]1)=[O:22]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH3:10])[CH2:11][C:12]1([CH2:13][CH2:14]2)[NH:15][C:16](=[O:17])[CH2:18][CH:19]([CH3:20])[C...
CCOC(=O)C1(NC(=O)CN(C)C(=O)OCc2ccccc2)CCc2cc(OC)c(OC)cc2C1
COc1cc2c(cc1OC)CC1(CC2)NC(=O)CC(C)C1=O
null
[Pd].[C]
null
Functional Group Interconversion
OtherReaction
1e566ba0eac3c52117da9c22073fbafe2426e0ffb781a46d21ae0e9ee9c169a8
ade0f728b01244fc6e52cce96c5fb074e8879beca54d54dd1088ee9c68307904
O=C1CCC(=O)C2(CCc3ccccc3C2)N1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[#7:4]-[C:5](=[O;D1;H0:6])-[CH2;D2;+0:7]-N(-[CH3;D1;+0:8])-C(=O)-O-C-c1:c:c:c:c:c:1)(-[C:9])-[C:10]>>[C:9]-[C:3]1(-[C:10])-[#7:4]-[C:5](=[O;D1;H0:6])-[CH2;D2;+0:7]-[C:11](-[CH3;D1;+0:8])-[C;H0;D3;+0:1]-1=[O;D1;H0:2]
null
[]
80
CELSIUS
null
null
A solution of ethyl 2-[(N-benzyloxycarbonyl-N-methylamino)acetylamino]-1,2,3,4-tetrahydro-6,7-dimethoxynaphthalene-2-carboxylate (550 mg, 1.1 mmol) in ethanol (20 ml) was hydrogenated in the presence of 10% Pd-carbon (250 mg) for 6 hr. The catalyst was filtered off and the filtrate was concentrated in vacuo. The residu...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ester.Ether
Ketone
c1ccccc1
c1ccc2c(c1)CCC1(CCCCN1)C2
c1ccc2c(c1)CCC1(CCCCN1)C2
HO-
[Pd].[C]
80
null
CCOC(=O)C1(NC(=O)CN(C)C(=O)OCc2ccccc2)CCc2cc(OC)c(OC)cc2C1>[Pd].[C]>COc1cc2c(cc1OC)CC1(CC2)NC(=O)CC(C)C1=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-de27506f180e47a2ad3ca470cfd3bc5a
COc1cc2c(cc1OC)CC1(CC2)NC(=O)CN(C)C1=O>>COc1cc2c(cc1OC)CC1(CC2)CN(C)CCN1
[OH-].[Na+].[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].COC=1C=C2CCC3(NC(CN(C3=O)C)=O)CC2=CC1OC>>COC=1C=C2CCC3(NCCN(C3)C)CC2=CC1OC
O=[C:15]1[C:12]2([CH2:11][c:6]3[c:5]([cH:4][c:3]([O:2][CH3:1])[c:8]([O:9][CH3:10])[cH:7]3)[CH2:14][CH2:13]2)[NH:20][C:19](=O)[CH2:18][N:16]1[CH3:17]>>[CH3:1][O:2][c:3]1[cH:4][c:5]2[c:6]([cH:7][c:8]1[O:9][CH3:10])[CH2:11][C:12]1([CH2:13][CH2:14]2)[CH2:15][N:16]([CH3:17])[CH2:18][CH2:19][NH:20]1
COc1cc2c(cc1OC)CC1(CC2)NC(=O)CN(C)C1=O
COc1cc2c(cc1OC)CC1(CC2)CN(C)CCN1
null
null
CCOCC
Reduction
OtherReaction
43346047900f30adf11967aa3aafab0638be00f3681f83791b2433d662065d71
1e111e1677c741c445104f499dde4d06874c64781551b41f18ee18795c631ec3
c1ccc2c(c1)CCC1(CNCCN1)C2
O=[C;H0;D3;+0:1]1-[#7:2](-[C;D1;H3:3])-[C:4]-[C;H0;D3;+0:5](=O)-[#7:6]-[C:7]-1(-[C:8])-[C:9]>>[C:8]-[C:7]1(-[C:9])-[#7:6]-[CH2;D2;+0:5]-[C:4]-[#7:2](-[C;D1;H3:3])-[CH2;D2;+0:1]-1
95
[{"value": 86.0, "product": "COC=1C=C2CCC3(NCCN(C3)C)CC2=CC1OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 95.0, "product": "COC=1C=C2CCC3(NCCN(C3)C)CC2=CC1OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
45
MINUTE
To a suspension of lithium aluminum hydride (114 mg, 3 mmol) and aluminum chloride (400 mg, 3 mmol) in ether (4 ml) was added the suspension of 3,4-dihydro-6,7-dimethoxy-4'-methylspiro[naphthalene-2(1H),2'-piperazine]-3',6'-dione (50 mg, 0.16 mmol) in ether (2 ml). The reaction mixture was stirred at ambient temperatur...
10.6084/m9.figshare.5104873.v1
null
Secondary amide.Tertiary amide
null
c1ccc2c(c1)CCC1(C[NH]CCN1)C2
c1ccc2c(c1)CCC1(C[NH]CCN1)C2
c1ccc2c(c1)CCC1(C[NH]CCN1)C2
Other
CCOCC
null
0.75
COc1cc2c(cc1OC)CC1(CC2)NC(=O)CN(C)C1=O>CCOCC>COc1cc2c(cc1OC)CC1(CC2)CN(C)CCN1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-8f22d5e763004e2ebbd516fb90970a8d
O=CNCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1>>NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1
C(=O)NCC(CCCN1CCC(CC1)C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[OH-].[Na+]>>NCC(CCCN1CCC(CC1)C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1
O=C[NH:1][CH2:2][C:3]([CH2:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([c:11]2[cH:12][cH:13][cH:14][cH:15][cH:16]2)[CH2:17][CH2:18]1)([c:19]1[cH:20][cH:21][cH:22][cH:23][cH:24]1)[c:25]1[cH:26][cH:27][cH:28][cH:29][cH:30]1>>[NH2:1][CH2:2][C:3]([CH2:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([c:11]2[cH:12][cH:13][cH:14]...
O=CNCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1
NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1
null
null
CO
Reduction
Reduction of primary amides to amines
755df58c254dea764fdda078ffd678ec540bba057c83683be04c253f1270ac7b
025f7cefe51e71668ad5d09fca32df168e9b538347403e4d5c1748073e538adc
c1ccc(C2CCN(CCCC(c3ccccc3)c3ccccc3)CC2)cc1
O=C-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
100.3
[{"value": 100.3, "product": "NCC(CCCN1CCC(CC1)C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 1-(5-formylamino-4,4-diphenylpentyl)-4-phenylpiperidine (2.07 g) in methanol (50 ml) was added 1N-sodium hydroxide (30 ml) and the mixture was refluxed overnight. This reaction mixture was concentrated to dryness and the group was extracted using methylene chloride and water. The organic layer was wash...
10.6084/m9.figshare.5104873.v1
null
Secondary amide
Primary amine
null
null
C1CC[NH]CC1.c1ccccc1.c1ccccc1.c1ccccc1
Other
CO
null
null
O=CNCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1>CO>NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-dd8d9889812644d1ab380e5a374a299b
COc1ccc2c(c1)CCC1(CCCCN1CCCC(CC#N)(c1ccccc1)c1ccccc1)C2>>COc1ccc2c(c1)CCC1(CCCCN1CCCC(CCN)(c1ccccc1)c1ccccc1)C2
[OH-].[Na+].COC=1C=C2CCC3(N(CCCC3)CCCC(CC#N)(C3=CC=CC=C3)C3=CC=CC=C3)CC2=CC1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O>>COC=1C=C2CCC3(N(CCCC3)CCCC(CCN)(C3=CC=CC=C3)C3=CC=CC=C3)CC2=CC1
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[CH2:9][CH2:10][C:11]1([CH2:12][CH2:13][CH2:14][CH2:15][N:16]1[CH2:17][CH2:18][CH2:19][C:20]([CH2:21][C:22]#[N:23])([c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1)[c:30]1[cH:31][cH:32][cH:33][cH:34][cH:35]1)[CH2:36]2>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[CH2:...
COc1ccc2c(c1)CCC1(CCCCN1CCCC(CC#N)(c1ccccc1)c1ccccc1)C2
COc1ccc2c(c1)CCC1(CCCCN1CCCC(CCN)(c1ccccc1)c1ccccc1)C2
null
null
O1CCCC1
Reduction
Reduction of nitrile to amine
65bec2d9f430701d30dc9fcbe1c5418f3dfa174d67be035c50edfc71895dc9c7
e8d1bc928b94bd4f5bf4b23363ce8f88b1ce7d146ba93829e7b8ad8dbe0007a7
c1ccc(C(CCCN2CCCCC23CCc2ccccc2C3)c2ccccc2)cc1
[C:1]-[C:2]-[C;H0;D2;+0:3]#[N;H0;D1;+0:4]>>[C:1]-[C:2]-[CH2;D2;+0:3]-[NH2;D1;+0:4]
89.2
[{"value": 89.2, "product": "COC=1C=C2CCC3(N(CCCC3)CCCC(CCN)(C3=CC=CC=C3)C3=CC=CC=C3)CC2=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
To a solution of 3,4-dihydro-6-methoxy-1'-(5-cyano-4,4-diphenylpentyl)spiro[naphthalene-2(1H),2'-piperidine] (0.6 g) in tetrahydrofuran (15 ml) was added lithium aluminum hydride (95 mg) portionwise under ice-cooling and stirring. After completion of dropwise addition, the mixture was heated at 60° C. for 6 hours. To t...
10.6084/m9.figshare.5104873.v1
null
Nitrile
Primary amine
null
null
c1ccc2c(c1)CCC1(CCCC[NH]1)C2.c1ccccc1.c1ccccc1
null
O1CCCC1
60
null
COc1ccc2c(c1)CCC1(CCCCN1CCCC(CC#N)(c1ccccc1)c1ccccc1)C2>O1CCCC1>COc1ccc2c(c1)CCC1(CCCCN1CCCC(CCN)(c1ccccc1)c1ccccc1)C2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-512e99f9a9254acd8ab4b706e0bfbb8f
CNC.O=CNCC(CCCI)(c1ccccc1)c1ccccc1>>CN(C)CCCC(CNC=O)(c1ccccc1)c1ccccc1
C(=O)NCC(CCCI)(C1=CC=CC=C1)C1=CC=CC=C1.Cl.CNC.C(C)N(CC)CC.C([O-])([O-])=O.[K+].[K+]>>CN(C)CCCC(CNC=O)(C1=CC=CC=C1)C1=CC=CC=C1
[CH3:1][NH:2][CH3:3].I[CH2:4][CH2:5][CH2:6][C:7]([CH2:8][NH:9][CH:10]=[O:11])([c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)[c:18]1[cH:19][cH:20][cH:21][cH:22][cH:23]1>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:5][CH2:6][C:7]([CH2:8][NH:9][CH:10]=[O:11])([c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1)[c:18]1[cH:19][cH:20][cH:21][cH:...
CNC.O=CNCC(CCCI)(c1ccccc1)c1ccccc1
CN(C)CCCC(CNC=O)(c1ccccc1)c1ccccc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
6d58cac08ccced0a33ed16fbca180bc12aa011288d6476106d98a7b2cbc3d709
523d37155b42c8dc851abeddadebb241cdd90bdf649ba750c35e13c8c752d7b0
c1ccc(Cc2ccccc2)cc1
I-[CH2;D2;+0:1]-[C:2]-[C:3].[C;D1;H3:4]-[NH;D2;+0:5]-[C;D1;H3:6]>>[C:3]-[C:2]-[CH2;D2;+0:1]-[N;H0;D3;+0:5](-[C;D1;H3:4])-[C;D1;H3:6]
67.1
[{"value": 67.1, "product": "CN(C)CCCC(CNC=O)(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 5-formylamino-1-iodo-4,4-diphenylpentane (8.5 g), dimethylamine hydrochloride (17.63 g), triethylamine (30.1 ml), and potassium carbonate (3 g) was heated in acetonitrile (250 ml) at 60° C. for 2 hours. This reaction mixture was concentrated to dryness and the group was extracted using ethyl acetate and wa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Secondary amine
Tertiary amine
null
null
c1ccccc1.c1ccccc1
HI
C(C)#N
null
null
CNC.O=CNCC(CCCI)(c1ccccc1)c1ccccc1>C(C)#N>CN(C)CCCC(CNC=O)(c1ccccc1)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-39787aa98c37454d9bfacfbb145e24ab
Cc1ccc(S(=O)(=O)NCC(CCCNCc2cccc([N+](=O)[O-])c2)(c2ccccc2)c2ccccc2)cc1>>Cc1ccc(S(=O)(=O)NCC(CCCNCc2cccc(N)c2)(c2ccccc2)c2ccccc2)cc1
C1(=CC=CC=C1)C(CCCNCC1=CC(=CC=C1)[N+](=O)[O-])(CNS(=O)(=O)C1=CC=C(C)C=C1)C1=CC=CC=C1.Cl>>NC=1C=C(CNCCCC(CNS(=O)(=O)C2=CC=C(C)C=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC1
O=[N+:22]([O-])[c:21]1[cH:20][cH:19][cH:18][c:17]([CH2:16][NH:15][CH2:14][CH2:13][CH2:12][C:11]([CH2:10][NH:9][S:6]([c:5]2[cH:4][cH:3][c:2]([CH3:1])[cH:37][cH:36]2)(=[O:7])=[O:8])([c:24]2[cH:25][cH:26][cH:27][cH:28][cH:29]2)[c:30]2[cH:31][cH:32][cH:33][cH:34][cH:35]2)[cH:23]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([S:6](=[O:7...
Cc1ccc(S(=O)(=O)NCC(CCCNCc2cccc([N+](=O)[O-])c2)(c2ccccc2)c2ccccc2)cc1
Cc1ccc(S(=O)(=O)NCC(CCCNCc2cccc(N)c2)(c2ccccc2)c2ccccc2)cc1
null
[Pd]
C(C)O
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=S(=O)(NCC(CCCNCc1ccccc1)(c1ccccc1)c1ccccc1)c1ccccc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
74.7
[{"value": 74.7, "product": "NC=1C=C(CNCCCC(CNS(=O)(=O)C2=CC=C(C)C=C2)(C2=CC=CC=C2)C2=CC=CC=C2)C=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4,4-diphenyl-1-(3-nitrobenzylamino)-5-(tosylamino)pentane (0.17 g) in ethanol (10 ml) was added hydrochloric acid (0.1 ml) as well as 10% palladium-on-carbon (80 mg) and the mixture was subjected to catalytic hydrogenation at atmospheric temperature and pressure. The catalyst was then removed from the ...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1.c1ccccc1.c1ccccc1
Other
[Pd].C(C)O
null
null
Cc1ccc(S(=O)(=O)NCC(CCCNCc2cccc([N+](=O)[O-])c2)(c2ccccc2)c2ccccc2)cc1>[Pd].C(C)O>Cc1ccc(S(=O)(=O)NCC(CCCNCc2cccc(N)c2)(c2ccccc2)c2ccccc2)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f481802e6a614778937029828a5a0491
CS(=O)(=O)Cl.NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1>>CS(=O)(=O)NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1.Cl
NCC(CCCN1CCC(CC1)C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.C(C)N(CC)CC.CS(=O)(=O)Cl>>Cl.C1(=CC=CC=C1)C(CCCN1CCC(CC1)C1=CC=CC=C1)(CNS(=O)(=O)C)C1=CC=CC=C1
[CH3:1][S:2](=[O:3])(=[O:4])[Cl:35].[NH2:5][CH2:6][C:7]([CH2:8][CH2:9][CH2:10][N:11]1[CH2:12][CH2:13][CH:14]([c:15]2[cH:16][cH:17][cH:18][cH:19][cH:20]2)[CH2:21][CH2:22]1)([c:23]1[cH:24][cH:25][cH:26][cH:27][cH:28]1)[c:29]1[cH:30][cH:31][cH:32][cH:33][cH:34]1>>[CH3:1][S:2](=[O:3])(=[O:4])[NH:5][CH2:6][C:7]([CH2:8][CH2:...
CS(=O)(=O)Cl.NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1
CS(=O)(=O)NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1.Cl
null
null
C(Cl)Cl
Miscellaneous
Sulfonamide synthesis (Schotten-Baumann) primary amine
a86b0632821e188c0a5dc5a5a2aac298ab3eccaee8a52ba46078c3d5975a290d
50f8fbf3d327483c3eeff8f6cbd4065e4c7600bb501fbe08958a5c79a0926428
c1ccc(C2CCN(CCCC(c3ccccc3)c3ccccc3)CC2)cc1
[C;D1;H3:1]-[S;H0;D4;+0:2](-[Cl;H0;D1;+0:3])(=[O;D1;H0:4])=[O;D1;H0:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[S;H0;D4;+0:2](-[C;D1;H3:1])(=[O;D1;H0:4])=[O;D1;H0:5].[ClH;D0;+0:3]
null
[]
null
null
null
null
To a solution of 5-amino-4,4-diphenyl-1-(4-phenylpiperidino)pentane (0.4 g) and triethylamine (0.42 ml) in methylene chloride (15 ml) was added methanesulfonyl chloride (0.1 ml) dropwise under ice-cooling and stirring. After completion of dropwise addition, the mixture was returned to room temperature and stirred for a...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Sulfonyl halide
Sulfonamide
null
null
C1CC[NH]CC1.c1ccccc1.c1ccccc1.c1ccccc1
null
C(Cl)Cl
null
null
CS(=O)(=O)Cl.NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1>C(Cl)Cl>CS(=O)(=O)NCC(CCCN1CCC(c2ccccc2)CC1)(c1ccccc1)c1ccccc1.Cl
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-206c74739b404c849cda9be7a167a4f0
N#CCCC(C=O)(c1ccccc1)c1ccccc1>>C=CC(O)C(CCC#N)(c1ccccc1)c1ccccc1
C1(=CC=CC=C1)C(CCC#N)(C=O)C1=CC=CC=C1.C(=C)[Mg]Br.O1CCCC1.[Cl-].[NH4+]>>C1(=CC=CC=C1)C(CCC#N)(C(C=C)O)C1=CC=CC=C1
[CH:3](=[O:4])[C:5]([CH2:6][CH2:7][C:8]#[N:9])([c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1>>[CH2:1]=[CH:2][CH:3]([OH:4])[C:5]([CH2:6][CH2:7][C:8]#[N:9])([c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[c:16]1[cH:17][cH:18][cH:19][cH:20][cH:21]1
N#CCCC(C=O)(c1ccccc1)c1ccccc1
C=CC(O)C(CCC#N)(c1ccccc1)c1ccccc1
null
null
O1CCCC1
Miscellaneous
OtherReaction
7c95c9d475b3e4739c4b4bffdb557ccc0332365664dc5f751958e7bb4139acbc
1cfdacde78204b273e664dc0eb50ffc4dc70522ea435514fcadd01e492b9b547
c1ccc(Cc2ccccc2)cc1
[C:1]-[C:2](-[c:3])(-[c:4])-[CH;D2;+0:5]=[O;H0;D1;+0:6]>>[C:1]-[C:2](-[c:3])(-[c:4])-[CH;D3;+0:5](-[OH;D1;+0:6])-[C:7]=[C;D1;H2:8]
null
[]
null
null
null
null
Under argon gas, 4,4-diphenyl-4-formylbutanenitrile (5.0 g) was dissolved in dry tetrahydrofuran (200 ml). Then, 1M vinylmagnesium bromide-tetrahydrofuran (30 ml) was added dropwise -40° C. After completion of addition, the reaction temperature was allowed to rise gradually to 0° C. (over 3 hours). After completion of ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol.Vinyl
null
null
c1ccccc1.c1ccccc1
Other
O1CCCC1
null
null
N#CCCC(C=O)(c1ccccc1)c1ccccc1>O1CCCC1>C=CC(O)C(CCC#N)(c1ccccc1)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-7124bdd5272a4ae488ccd70f9adb1d70
N[C@@H](CCC(=O)O)C(=O)O.Nc1ccc(S(=O)(=O)O)cc1.O=C(O)/C=C\C(=O)O.O=C(O)[C@@H]1CCCN1>>C1COCCN1.CCCCN.CCCN
C(\C=C/C(=O)O)(=O)O.C1(\C=C/C(=O)O1)=O.NCC(=O)O.N[C@@H](CCC(=O)O)C(=O)O.N[C@@H](C)C(=O)O.N1[C@H](C(=O)O)CCC1.C(C=1C(N)=CC=CC1)(=O)O.C1(\C=C/C(=O)O1)=O.S(=O)(C1=CC=C(C=C1)N)(=O)O.NC1=C(C(=CC=C1)C)S(=O)(=O)O.C=1C=CC=2C=C(C=CC2C1)N.C=1C=CC=2C=C(C=CC2C1)N>>C1(\C=C/C(=O)O1)=O.C(CC)N.C(CCC)N.N1CCOCC1
O=C(O)CC[C@@H](C(=O)O)[NH2:6].O=S(=O)(O)[c:7]1[cH:4][cH:5][c:10]([NH2:11])[cH:9][cH:8]1.O=C(O)/C=[CH:1]\[C:2](=O)[OH:3].O=C(O)[C@@H]1[CH2:12][CH2:13][CH2:14][NH:15]1>>[CH2:1]1[CH2:2][O:3][CH2:4][CH2:5][NH:6]1.[CH3:7][CH2:8][CH2:9][CH2:10][NH2:11].[CH3:12][CH2:13][CH2:14][NH2:15]
N[C@@H](CCC(=O)O)C(=O)O.Nc1ccc(S(=O)(=O)O)cc1.O=C(O)/C=C\C(=O)O.O=C(O)[C@@H]1CCCN1
C1COCCN1.CCCCN.CCCN
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
9ef43ec893906d526b8efc2c8f7bd766d08677a08736af6c7264afc1ae0701cd
b21ff3392680300b41449088b20ca9844ed9d399d436929809148c0373cac5ed
C1COCCN1
O-C(=O)-C-C-[C@@H](-[NH2;D1;+0:1])-C(-O)=O.O-C(=O)-[C@H]1-[CH2;D2;+0:2]-[C:3]-[C:4]-[NH;D2;+0:5]-1.O-C(=O)/C=[CH;D2;+0:6]\[C;H0;D3;+0:7](=O)-[OH;D1;+0:8].O-S(=O)(=O)-[c;H0;D3;+0:9]1:[cH;D2;+0:10]:[cH;D2;+0:11]:[c;H0;D3;+0:12](-[N;D1;H2:13]):[cH;D2;+0:14]:[cH;D2;+0:15]:1>>[CH2;D2;+0:6]1-[CH2;D2;+0:7]-[O;H0;D2;+0:8]-[CH2...
null
[]
null
null
null
null
Examples of monomers which can provide structure units represented by Formula (4) include half amides of maleic acid, prepared by the reaction of maleic anhydride with glycine, glutamic acid, alanine, proline, anthranilic acid or by the reaction of maleic anhydride with sulfanilic acid, amino-toluene sulfonic acid, nap...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Carboxylic acid.Carboxylic acid.Carboxylic acid.Carboxylic acid.Primary amine.Secondary amine.Sulfonic acid
Ether.Primary amine.Secondary amine
c1ccccc1.C1CCNC1
C1COCCN1
C1COCCN1
Other
null
null
null
N[C@@H](CCC(=O)O)C(=O)O.Nc1ccc(S(=O)(=O)O)cc1.O=C(O)/C=C\C(=O)O.O=C(O)[C@@H]1CCCN1>>C1COCCN1.CCCCN.CCCN
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3b264efffb7c4bf6baad7d517a038167
CC(C)(C)[Si](C)(C)Cl.COC(=O)CC/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>>COC(=O)CC/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
O.OC1=C2C(OCC2=C(C(=C1C/C=C(/CCC(=O)OC)\C)OC)C)=O.[Si](C)(C)(C(C)(C)C)Cl.N1C=NC=C1>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/CCC(=O)OC)\C)OC)C)=O
Cl[Si:21]([CH3:22])([CH3:23])[C:24]([CH3:25])([CH3:26])[CH3:27].[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6]/[C:7]([CH3:8])=[CH:9]/[CH2:10][c:11]1[c:12]([O:13][CH3:14])[c:15]([CH3:16])[c:17]2[c:18]([c:19]1[OH:20])[C:28](=[O:29])[O:30][CH2:31]2>>[CH3:1][O:2][C:3](=[O:4])[CH2:5][CH2:6]/[C:7]([CH3:8])=[CH:9]/[CH2:10][c:11]1[c:...
CC(C)(C)[Si](C)(C)Cl.COC(=O)CC/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
COC(=O)CC/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
null
CN(C=O)C
Protection
Alcohol protection with silyl ethers
91043baed1393f1ecd2302d7d0b31c01cf171d3977dd7c70afa1da52fa298c73
4a917c959d011f885a1269fa3c1f022ee5e09144996246d24e42e65634a451ac
O=C1OCc2ccccc21
Cl-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[#8:8]-[C:9](=[O;D1;H0:10])-[c:11]:[c:12](-[OH;D1;+0:13]):[c:14]>>[#8:8]-[C:9](=[O;D1;H0:10])-[c:11]:[c:12](-[O;H0;D2;+0:13]-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7]):[c:14]
null
[]
50
CELSIUS
24
HOUR
To methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl) -4-methyl-4-hexenoate (Tetrahedron, 28, 4395, 1972) (10.0 g) in dimethylformamide (75 ml) was added t-butyldimethylsilyl chloride (4.97 g) and imidazole (2.24 g). The mixture was heated at 50° C. for 1 hour, then left at room temperature...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol.Silyl protective group
TMS ether protective group
null
null
c1ccc2c(c1)COC2
HCl
CN(C=O)C
50
24
CC(C)(C)[Si](C)(C)Cl.COC(=O)CC/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>CN(C=O)C>COC(=O)CC/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-dfb5a7b7973c4b7fbba91920cc2aedaa
COC(=O)CC/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O.COCCOCCl>>COCCOCOc1c(C/C=C(\C)CCC(=O)OC)c(OC)c(C)c2c1C(=O)OC2
OC1=C2C(OCC2=C(C(=C1C/C=C(/CCC(=O)OC)\C)OC)C)=O.C(C)(C)N(CC)C(C)C.COCCOCCl>>COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CCC(=O)OC)\C
[OH:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH2:14][CH2:15][C:16](=[O:17])[O:18][CH3:19])[c:20]([O:21][CH3:22])[c:23]([CH3:24])[c:25]2[c:26]1[C:27](=[O:28])[O:29][CH2:30]2.Cl[CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH2:14]...
COC(=O)CC/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O.COCCOCCl
COCCOCOc1c(C/C=C(\C)CCC(=O)OC)c(OC)c(C)c2c1C(=O)OC2
null
null
C(Cl)Cl
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
6e90ffbf0683e1a3ee55c5e3ea453aefc5ddd369c0150ed0150f9546d7e47f4f
efd670663709b79afcad1306da9f69b33a0147cfa3639ca4c0b54b35ef4b1852
O=C1OCc2ccccc21
Cl-[CH2;D2;+0:1]-[#8:2]-[C:3].[#8:4]-[C:5](=[O;D1;H0:6])-[c:7]:[c:8](-[OH;D1;+0:9]):[c:10]>>[#8:4]-[C:5](=[O;D1;H0:6])-[c:7]:[c:8](-[O;H0;D2;+0:9]-[CH2;D2;+0:1]-[#8:2]-[C:3]):[c:10]
null
[]
null
null
null
null
To methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoate (61.0 g) in methylene chloride (1000 ml) at 0° C. was added diisopropylethylamine (30.4 g) and methoxyethoxymethyl chloride (29.2 g). After 31/2 hours the solution was washed with dilute hydrochloric acid, dried and ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ether.Aromatic alcohol
Ether.Ether
null
null
c1ccc2c(c1)COC2
HCl
C(Cl)Cl
null
null
COC(=O)CC/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O.COCCOCCl>C(Cl)Cl>COCCOCOc1c(C/C=C(\C)CCC(=O)OC)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-782f3ef968454e2fb4c7a53a51cbf910
COC(=O)CC/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC=O)C(=O)OC2
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/CCC(=O)OC)\C)OC)C)=O.ClCCl.N1=CC=CC=C1.CO>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1CC=O)OC)C)=O
COC(CC/C(C)=[CH:19]/[CH2:18][c:17]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[O:9][Si:10]([CH3:11])([CH3:12])[C:13]([CH3:14])([CH3:15])[CH3:16])[C:21](=[O:22])[O:23][CH2:24]2)=[O:20]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][Si:10]([CH3:11])([CH3:12])[C:13]([CH3:14])([CH3:15])[CH3:16])[c:17]1[CH...
COC(=O)CC/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC=O)C(=O)OC2
null
null
null
Miscellaneous
Alkene oxidation to aldehyde
bead50fbe5f064ca194dd6539169819285be7ad836d4784cf731500fc82ffd81
4c6528619563bcf8307b99ed5b55eeec359e10edc84b38b6723a7f0e61ea5d01
O=C1OCc2ccccc21
C-O-C(=[O;H0;D1;+0:1])-C-C/C(-C)=[CH;D2;+0:2]/[C:3]-[c:4]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[C:3]-[c:4]
null
[]
null
null
45
MINUTE
A solution of methyl (E)-6-(4-t-butyldimethylsilyloxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoate (11.0 g) in methanol 125 ml), dichloromethane (125 ml) and pyridine (2 ml) was cooled to -78° C. and a stream of ozonized oxygen was bubbled through. After 45 minutes a blue color developed...
10.6084/m9.figshare.5104873.v1
null
Ester
Aldehyde
null
null
c1ccc2c(c1)COC2
HO-
null
null
0.75
COC(=O)CC/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC=O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ea17c53062cd4009bf12f9a094220e13
COCCOCOc1c(C/C=C(\C)CCC(=O)OC)c(OC)c(C)c2c1C(=O)OC2>>COCCOCOc1c(C/C=C(\C)CCC(=O)O)c(OC)c(C)c2c1C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CCC(=O)OC)\C.[OH-].[Na+]>>COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CCC(=O)O)\C
C[O:18][C:16]([CH2:15][CH2:14]/[C:12](=[CH:11]/[CH2:10][c:9]1[c:8]([O:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[c:25]2[c:24]([c:22]([CH3:23])[c:19]1[O:20][CH3:21])[CH2:29][O:28][C:26]2=[O:27])[CH3:13])=[O:17]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH2:14][CH2:15][C:16...
COCCOCOc1c(C/C=C(\C)CCC(=O)OC)c(OC)c(C)c2c1C(=O)OC2
COCCOCOc1c(C/C=C(\C)CCC(=O)O)c(OC)c(C)c2c1C(=O)OC2
null
null
O.CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccccc21
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
To methyl (E)-6-(1,3-dihydro-6-methoxy -4-methoxyethoxymethoxy-7-methyl-3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoate (76.0 g) in methanol (300 ml) was added 1N aqueous sodium hydroxide (300 ml). After 11/2 hours the solution was diluted with water, washed twice with ether, then acidified with dilute hydrochloric acid....
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccc2c(c1)COC2
Other
O.CO
null
null
COCCOCOc1c(C/C=C(\C)CCC(=O)OC)c(OC)c(C)c2c1C(=O)OC2>O.CO>COCCOCOc1c(C/C=C(\C)CCC(=O)O)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9c6929ae720b47be8f9702cfd7e578b5
COCCOCOc1c(C/C=C(\C)CCC(=O)O)c(OC)c(C)c2c1C(=O)OC2>>COCCOCOc1c(CC=O)c(OC)c(C)c2c1C(=O)OC2
CCCCCC.C(C)(=O)OCC.COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CCC(=O)O)\C>>COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)CC=O
C/C(CCC(=O)[OH:12])=[CH:11]\[CH2:10][c:9]1[c:8]([O:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[c:19]2[c:18]([c:16]([CH3:17])[c:13]1[O:14][CH3:15])[CH2:23][O:22][C:20]2=[O:21]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10][CH:11]=[O:12])[c:13]([O:14][CH3:15])[c:16]([CH3:17])[c:18]2[c:19]1[C:20](=[O:21])[...
COCCOCOc1c(C/C=C(\C)CCC(=O)O)c(OC)c(C)c2c1C(=O)OC2
COCCOCOc1c(CC=O)c(OC)c(C)c2c1C(=O)OC2
null
null
null
Miscellaneous
Alkene oxidation to aldehyde
148369763d5ac94fa638d0416b05b2817b88fbcf3e3881a34df5b1c1422931df
8efb0e76025bf10ceb3c462bb2943eb84b6953d35e82203a100aa1bb9e5b03cd
O=C1OCc2ccccc21
C/C(-C-C-C(=O)-[OH;D1;+0:1])=[CH;D2;+0:2]\[C:3]-[c:4]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[C:3]-[c:4]
null
[]
null
null
null
null
By following the procedure of part A and substituting methyl (E)-6-(4-t-butyldimethylsilyloxy-1,3-dihydro -6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoate with (E)-6-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy-7-methyl -3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoic acid, there was obtained 2-(1,3-dihy...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Aldehyde
null
null
c1ccc2c(c1)COC2
HO-
null
null
null
COCCOCOc1c(C/C=C(\C)CCC(=O)O)c(OC)c(C)c2c1C(=O)OC2>>COCCOCOc1c(CC=O)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f078921265d0411fa08bc67cd49cab1e
C=C(C)C(O)Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>COC(=O)C(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1CC(C(=C)C)O)OC)C)=O>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OC)C)\C)OC)C)=O
[CH3:1][C:25]([Si:22]([O:21][c:20]1[c:12]([CH2:11][CH:10]([OH:2])[C:8](=[CH2:7])[CH3:9])[c:13]([O:14][CH3:15])[c:16]([CH3:17])[c:18]2[c:19]1[C:29](=[O:30])[O:31][CH2:32]2)([CH3:23])[CH3:24])([CH3:26])[CH3:28]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH3:6])[CH2:7]/[C:8]([CH3:9])=[CH:10]/[CH2:11][c:12]1[c:13]([O:14][CH3:15])[c...
C=C(C)C(O)Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
COC(=O)C(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
null
C(CC)(OC)(OC)OC.C(CC)(=O)O
Functional Group Addition
OtherReaction
95879aa68e13a7c3887b644a0e5ab788bc8ccac1864a8b46ceb70548db1d9693
c35876feeb8f837edfa28d6fabc0bcd11e4c5bd63ed79647940225e1df640f0b
O=C1OCc2ccccc21
[#8:1]-[#14:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[C;H0;D4;+0:5](-[C;D1;H3:6])(-[C;D1;H3:7])-[CH3;D1;+0:8].[C;D1;H3:9]-[C;H0;D3;+0:10](=[CH2;D1;+0:11])-[CH;D3;+0:12](-[OH;D1;+0:13])-[C:14]-[c:15]>>[#8:1]-[#14:2](-[C;D1;H3:3])(-[C;D1;H3:4])-[C;H0;D4;+0:5](-[C;D1;H3:6])(-[C;D1;H3:16])-[C;D1;H3:7].[C;D1;H3:17]-[C:18](-[CH2;D2;+0...
null
[]
null
null
null
null
A solution of 4-(4-tert-butyldimethylsilyloxy-1,3-dihydro-6-methoxy -7-methyl-3-oxoisobenzofuran-5-yl)-3-hydroxy-2-methylbut-1-ene (0.91 g) in trimethyl orthopropionate (25 ml) and propionic acid (0.08 ml) was heated to 110° C. for 2.5 hours. The solvents were evaporated under vacuum to afford methyl (E)-6-(4-tert-buty...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Vinyl.TMS ether protective group
Ester.TMS ether protective group
null
null
c1ccc2c(c1)COC2
Other
C(CC)(OC)(OC)OC.C(CC)(=O)O
null
null
C=C(C)C(O)Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>C(CC)(OC)(OC)OC.C(CC)(=O)O>COC(=O)C(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4e1328b28d1a47029e53dfd91f1f4ad0
COC(=O)C(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>COC(=O)C(C)C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OC)C)\C)OC)C)=O.[F-].C(CCC)[N+](CCCC)(CCCC)CCCC>>OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OC)C)\C)OC)C)=O
CC(C)(C)[Si](C)(C)[O:14][c:13]1[c:12]([CH2:11]/[CH:10]=[C:8](/[CH2:7][CH:5]([C:3]([O:2][CH3:1])=[O:4])[CH3:6])[CH3:9])[c:19]([O:20][CH3:21])[c:17]([CH3:18])[c:16]2[c:15]1[C:24](=[O:25])[O:23][CH2:22]2>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH3:6])[CH2:7]/[C:8]([CH3:9])=[CH:10]/[CH2:11][c:12]1[c:13]([OH:14])[c:15]2[c:16]([c:...
COC(=O)C(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
COC(=O)C(C)C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
null
null
O1CCCC1
Deprotection
Alcohol deprotection from silyl ethers
e70131badc7d7d580ed75b2dfb3ce6df2a5f496b2119611cf5354e1267babe73
b09ece7bccc3ff762f4ff5407ad846fffba6d6a63735853c86a86d29904f54ed
O=C1OCc2ccccc21
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](=[O;D1;H0:6])-[#8:7]>>[#8:7]-[C:5](=[O;D1;H0:6])-[c:4]:[c:2](-[OH;D1;+0:1]):[c:3]
null
[]
null
null
null
null
To methyl (E)-6-(4-tert-butyldimethylsilyloxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2,4-dimethyl-4-hexenoate (0.8 g) in tetrahydrofuran (5 ml) was added 1N tetra-n-butylammonium fluoride in tetrahydrofuran (4 ml). After 10 minutes the solution was diluted with ice water and extracted with ethyl acetat...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Aromatic alcohol
null
null
c1ccc2c(c1)COC2
Other
O1CCCC1
null
null
COC(=O)C(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>O1CCCC1>COC(=O)C(C)C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-72415126fa004050bfea8158ceb7782c
COC(=O)C(C)C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>>COc1c(C)c2c(c(O)c1C/C=C(\C)CC(C)C(=O)O)C(=O)OC2
Cl.OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OC)C)\C)OC)C)=O.[OH-].[Li+]>>OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)O)C)\C)OC)C)=O
C[O:20][C:18]([CH:16]([CH2:15]/[C:13](=[CH:12]/[CH2:11][c:10]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[OH:9])[C:21](=[O:22])[O:23][CH2:24]2)[CH3:14])[CH3:17])=[O:19]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11]/[CH:12]=[C:13](\[CH3:14])[CH2:15][CH:16]([CH3:17])[C:18](=[O:19])[OH:...
COC(=O)C(C)C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
COc1c(C)c2c(c(O)c1C/C=C(\C)CC(C)C(=O)O)C(=O)OC2
null
null
O.CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccccc21
C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
4
HOUR
To methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2,4-dimethyl-4-hexenoate (0.85 g) in methanol (10 ml) was added a solution of lithium hydroxide (0.4 g) in water (5 ml). After 4 hours at room temperature, the solution was poured into ice water, acidified with 10% aqueous hydrochloric a...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccc2c(c1)COC2
Other
O.CO
null
4
COC(=O)C(C)C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>O.CO>COc1c(C)c2c(c(O)c1C/C=C(\C)CC(C)C(=O)O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4f4f7c5bfbac4cb282ab0edfc243fca8
CC(C=O)=P(c1ccccc1)(c1ccccc1)c1ccccc1.COCCOCOc1c(CC=O)c(OC)c(C)c2c1C(=O)OC2>>COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)CC=O.C1(=CC=CC=C1)P(=C(C=O)C)(C1=CC=CC=C1)C1=CC=CC=C1>>COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/C=O)\C
c1ccc(P(c2ccccc2)(c2ccccc2)=[C:12]([CH3:13])[CH:14]=[O:15])cc1.O=[CH:11][CH2:10][c:9]1[c:8]([O:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[c:22]2[c:21]([c:19]([CH3:20])[c:16]1[O:17][CH3:18])[CH2:26][O:25][C:23]2=[O:24]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH:14]=[O:15...
CC(C=O)=P(c1ccccc1)(c1ccccc1)c1ccccc1.COCCOCOc1c(CC=O)c(OC)c(C)c2c1C(=O)OC2
COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2
null
null
C1(=CC=CC=C1)C
C-C Coupling
Wittig reaction with triphenylphosphorane
ba14f60c8faf1e2b5d258488ef5e81c88d381e470a98a19e511c94a7a3104695
3174a51604157c488f07402e36f994f716989b8fc10687ee243713b4cfbdb11a
O=C1OCc2ccccc21
O=[CH;D2;+0:1]-[C:2]-[c:3].[C;D1;H3:4]-[C;H0;D3;+0:5](-[C:6]=[O;D1;H0:7])=P(-c1:c:c:c:c:c:1)(-c1:c:c:c:c:c:1)-c1:c:c:c:c:c:1>>[C;D1;H3:4]/[C;H0;D3;+0:5](-[C:6]=[O;D1;H0:7])=[CH;D2;+0:1]\[C:2]-[c:3]
null
[]
null
null
null
null
A solution of 2-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy -7-methyl-3-oxoisobenzofuran-5-yl)acetaldehyde (10.3 g) and 2-(triphenyl-phosphoranylidene)-propionaldehyde (11.6 g) in toluene (250 ml) was refluxed for 7 hours. The solvent was removed under vacuum and the residue was chromatographed on silica gel, eluting...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Aldehyde
Aldehyde
c1ccccc1.c1ccccc1.c1ccccc1
null
c1ccc2c(c1)COC2
HO-
C1(=CC=CC=C1)C
null
null
CC(C=O)=P(c1ccccc1)(c1ccccc1)c1ccccc1.COCCOCOc1c(CC=O)c(OC)c(C)c2c1C(=O)OC2>C1(=CC=CC=C1)C>COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-5345bf2b94bc498b82d222f982316189
CCOC(=O)C(C)C.COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2>>CCOC(=O)C(C)(C)C(O)/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/C=O)\C.C(C)(C)NC(C)C.[Li]CCCC.[NH4+].[Cl-].C(C(C)C)(=O)OCC>>COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/C(C(C(=O)OCC)(C)C)O)\C)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH3:7])[CH3:8].[CH:9](=[O:10])/[C:11]([CH3:12])=[CH:13]/[CH2:14][c:15]1[c:16]([O:17][CH3:18])[c:19]([CH3:20])[c:21]2[c:22]([c:23]1[O:24][CH2:25][O:26][CH2:27][CH2:28][O:29][CH3:30])[C:31](=[O:32])[O:33][CH2:34]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[CH:9]([OH:1...
CCOC(=O)C(C)C.COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2
CCOC(=O)C(C)(C)C(O)/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
null
null
C1CCOC1
C-C Coupling
Aldol condensation
5c727118385c562f285df4622fd28beee54f2a6dc613daeca0713283cec89087
12ce375342f37362e14813852abaca485261821306a77d2d6bbedf8a6a5866f3
O=C1OCc2ccccc21
[C;D1;H3:1]/[C:2](=[C:3]\[C:4]-[c:5])-[CH;D2;+0:6]=[O;H0;D1;+0:7].[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[CH;D3;+0:12](-[C;D1;H3:13])-[C;D1;H3:14]>>[C:8]-[#8:9]-[C:10](=[O;D1;H0:11])-[C;H0;D4;+0:12](-[C;D1;H3:13])(-[C;D1;H3:14])-[CH;D3;+0:6](-[OH;D1;+0:7])/[C:2](-[C;D1;H3:1])=[C:3]/[C:4]-[c:5]
87
[{"value": 87.0, "product": "COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/C(C(C(=O)OCC)(C)C)O)\\C)OC)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
20
MINUTE
Freshly distilled diisopropylamine (0.425 ml) was dissolved in anhydrous THF (10 ml) and cooled to 0° C. n-BuLi (0.63 ml, 2.35M) was added slowly and the reaction was stirred at 0° C. for 20 minutes and cooled to -78°. Ethyl isobutyrate (0.200 ml) was added and the resulting solution was stirred at -78° C. for 40 minut...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester
Ester.Secondary alcohol
null
null
c1ccc2c(c1)COC2
null
C1CCOC1
0
0.333333
CCOC(=O)C(C)C.COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2>C1CCOC1>CCOC(=O)C(C)(C)C(O)/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-c8fe2bc179014416806c17e5f7ee215d
CCOC(=O)C(C)(C)C(O)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>>COc1c(C)c2c(c(O)c1C/C=C(\C)C(O)C(C)(C)C(=O)O)C(=O)OC2
OC1=C2C(OCC2=C(C(=C1C/C=C(/C(C(C(=O)OCC)(C)C)O)\C)OC)C)=O>>OC1=C2C(OCC2=C(C(=C1C/C=C(/C(C(C(=O)O)(C)C)O)\C)OC)C)=O
CC[O:22][C:20]([C:17]([CH:15](/[C:13](=[CH:12]/[CH2:11][c:10]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[OH:9])[C:23](=[O:24])[O:25][CH2:26]2)[CH3:14])[OH:16])([CH3:18])[CH3:19])=[O:21]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11]/[CH:12]=[C:13](\[CH3:14])[CH:15]([OH:16])[C:17]([CH...
CCOC(=O)C(C)(C)C(O)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
COc1c(C)c2c(c(O)c1C/C=C(\C)C(O)C(C)(C)C(=O)O)C(=O)OC2
null
null
CCOCC.C(C)(=O)OCC
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccccc21
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
By following the procedure of Example ZA-6A and substituting methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl) 2,4-dimethyl-4-hexenoate with ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2,2,4-trimethyl-3-hydroxy-4-hexenoate and the corresponding compounds ...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccc2c(c1)COC2
Other
CCOCC.C(C)(=O)OCC
null
null
CCOC(=O)C(C)(C)C(O)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>CCOCC.C(C)(=O)OCC>COc1c(C)c2c(c(O)c1C/C=C(\C)C(O)C(C)(C)C(=O)O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-80a07f86bd5b4e04b69809945bd1ada7
CCOC(=O)CC(O)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.CI>>CCOC(=O)CC(OC)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)O)\C)OC)C)=O.CI>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)OC)\C)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]([OH:8])/[C:10]([CH3:11])=[CH:12]/[CH2:13][c:14]1[c:15]([O:16][CH3:17])[c:18]([CH3:19])[c:20]2[c:21]([c:22]1[O:23][Si:24]([CH3:25])([CH3:26])[C:27]([CH3:28])([CH3:29])[CH3:30])[C:31](=[O:32])[O:33][CH2:34]2.I[CH3:9]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]([O:8][CH3:9]...
CCOC(=O)CC(O)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.CI
CCOC(=O)CC(OC)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
[Ag]=O
CC#N
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
31ec8f945a35f4f87287620e27b68692ce42732551035fbac056df61d9acce14
08f7221cae607d413f579138dcaa6997bebcad2bbb42d2f1b3b2a2d886befb37
O=C1OCc2ccccc21
I-[CH3;D1;+0:1].[#8:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6](-[OH;D1;+0:7])/[C:8](-[C;D1;H3:9])=[C:10]/[C:11]>>[#8:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6](-[O;H0;D2;+0:7]-[CH3;D1;+0:1])/[C:8](-[C;D1;H3:9])=[C:10]/[C:11]
60
[{"value": 60.0, "product": "[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)OC)\\C)OC)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Ethyl (E)-6-(1,3-dihydro-4-tert -butyldimethylsilyloxy-6-methoxy -7-methyl-3-oxoisobenzofuran-5-yl)-3-hydroxy-4-methyl-4-hexenoate (974 mg) was dissolved in a 6:1 mixture of methyl iodide in CH3CN (25 ml). Silver oxide was then added (5.1 g) and the mixture heated at reflux for 24 hr. The mixture was cooled to room tem...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ether
null
null
c1ccc2c(c1)COC2
HI
[Ag]=O.CC#N
null
null
CCOC(=O)CC(O)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.CI>[Ag]=O.CC#N>CCOC(=O)CC(OC)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-78e66f63118845168ca11d31beeffab3
CCOC(=O)CC(OC)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>>COc1c(C)c2c(c(O)c1C/C=C(\C)C(CC(=O)O)OC)C(=O)OC2
OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)OC)\C)OC)C)=O>>OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)O)OC)\C)OC)C)=O
CC[O:19][C:17]([CH2:16][CH:15](/[C:13](=[CH:12]/[CH2:11][c:10]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[OH:9])[C:22](=[O:23])[O:24][CH2:25]2)[CH3:14])[O:20][CH3:21])=[O:18]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11]/[CH:12]=[C:13](\[CH3:14])[CH:15]([CH2:16][C:17](=[O:18])[OH:19...
CCOC(=O)CC(OC)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
COc1c(C)c2c(c(O)c1C/C=C(\C)C(CC(=O)O)OC)C(=O)OC2
null
null
CCCCCC.C(Cl)Cl
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccccc21
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
By following the procedure of Example ZA-6A and substituting methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl) 2,4-dimethyl-4-hexenoate with ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-3-methoxy-4-methyl-4-hexenoate and the corresponding compounds of Form...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccc2c(c1)COC2
Other
CCCCCC.C(Cl)Cl
null
null
CCOC(=O)CC(OC)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>CCCCCC.C(Cl)Cl>COc1c(C)c2c(c(O)c1C/C=C(\C)C(CC(=O)O)OC)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1cab9284e0e142118725aa659befdec5
COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2>>COCCOCOc1c(C/C=C(\C)CO)c(OC)c(C)c2c1C(=O)OC2
O.COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/C=O)\C.[BH4-].[Na+]>>COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CO)\C
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH:14]=[O:15])[c:16]([O:17][CH3:18])[c:19]([CH3:20])[c:21]2[c:22]1[C:23](=[O:24])[O:25][CH2:26]2>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH2:14][OH:15])[c:16]([O:17][CH3:18])[c:19...
COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2
COCCOCOc1c(C/C=C(\C)CO)c(OC)c(C)c2c1C(=O)OC2
null
null
CO
Reduction
Reduction of aldehydes and ketones to alcohols
e7895795cd3f75445716c94697823c5929dcd4b5344525875fe75d36bca2f9d7
21bb81d5469aaaca71ab12c186bea4016451717fad8780cf288858a7d8fbc55a
O=C1OCc2ccccc21
[C;D1;H3:1]/[C:2](=[C:3]\[C:4]-[c:5])-[CH;D2;+0:6]=[O;H0;D1;+0:7]>>[C;D1;H3:1]/[C:2](=[C:3]\[C:4]-[c:5])-[CH2;D2;+0:6]-[OH;D1;+0:7]
null
[]
null
null
null
null
To a solution of (E)-4-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-methylbut-2-enaldehyde (4.6 g) in methanol (60 ml) was added sodium borohydride (0.528 g). After one hour the reaction was added to water (250 ml) and extracted with ethyl acetate (2×150 ml). The extract was dried a...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Primary alcohol
null
null
c1ccc2c(c1)COC2
null
CO
null
null
COCCOCOc1c(C/C=C(\C)C=O)c(OC)c(C)c2c1C(=O)OC2>CO>COCCOCOc1c(C/C=C(\C)CO)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3d832c1fcf3c483f83810b22f9dee1dd
COCCOCOc1c(C/C=C(\C)CO)c(OC)c(C)c2c1C(=O)OC2.O=C1CCC(=O)N1Br>>COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2
BrN1C(CCC1=O)=O.COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CO)\C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CBr)\C
O[CH2:14]/[C:12](=[CH:11]/[CH2:10][c:9]1[c:8]([O:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[c:22]2[c:21]([c:19]([CH3:20])[c:16]1[O:17][CH3:18])[CH2:26][O:25][C:23]2=[O:24])[CH3:13].O=C1CCC(=O)N1[Br:15]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[CH2:14][Br:15])[c:16]([O:17]...
COCCOCOc1c(C/C=C(\C)CO)c(OC)c(C)c2c1C(=O)OC2.O=C1CCC(=O)N1Br
COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2
null
null
C(Cl)Cl
Functional Group Interconversion
OtherReaction
f5aab884336f72e1370119b83151f1b95e31e5f052f259aee44382a5b9c14686
2aeb112456268e3e5dab065a03bb8fc4b6e8f1d07cae05ef26dce278613b654e
O=C1OCc2ccccc21
O-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6].O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:7]>>[Br;H0;D1;+0:7]-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6]
null
[]
null
null
null
null
To a solution of (E)-4-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-methylbut-2-en-1-ol (4.6 g) in methylene chloride (100 ml) at 0° C. was added triphenylphosphine (3.64 g) then N-bromosuccinimide (2.48 g). After 15 minutes the solution was washed with 10% aqueous sodium bisulphite...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide.Primary alcohol
Primary halide
C1CCNC1
null
c1ccc2c(c1)COC2
HO-
C(Cl)Cl
null
null
COCCOCOc1c(C/C=C(\C)CO)c(OC)c(C)c2c1C(=O)OC2.O=C1CCC(=O)N1Br>C(Cl)Cl>COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-974ff8f64ce5424998e02f92638f72db
CCOC(C)=O.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2.[NH4+]>>CCOC(=O)C(N)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
[NH4+].[Cl-].COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CBr)\C.C(C)(=O)OCC.[Li]CCCC.C(C)(C)NC(C)C>>COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)N)\C)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH3:6].Br[CH2:8]/[C:9]([CH3:10])=[CH:11]/[CH2:12][c:13]1[c:14]([O:15][CH3:16])[c:17]([CH3:18])[c:19]2[c:20]([c:21]1[O:22][CH2:23][O:24][CH2:25][CH2:26][O:27][CH3:28])[C:29](=[O:30])[O:31][CH2:32]2.[NH4+:7]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([NH2:7])[CH2:8]/[C:9]([CH3:10])=[CH:11]/[...
CCOC(C)=O.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2.[NH4+]
CCOC(=O)C(N)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
null
null
CN(C)P(=O)(N(C)C)N(C)C.C1CCOC1
Heteroatom Alkylation and Arylation
OtherReaction
021424c3b860edcb551eeea16c22a1ab914c9407329c37932b427a0488e708d5
4ccd83de18159de0cdb89422fce5446da660f78eea0800945f87eaa501327824
O=C1OCc2ccccc21
Br-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6].[C:7]-[#8:8]-[C:9](-[CH3;D1;+0:10])=[O;D1;H0:11].[NH4+;D0:12]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:11])-[CH;D3;+0:10](-[NH2;D1;+0:12])-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6]
63
[{"value": 63.0, "product": "COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)N)\\C)OC)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
20
MINUTE
Freshly distilled diisopropylamine (0.435 ml) was dissolved in THF (10 ml). The solution was cooled to 0° C. and n-BuLi (1.3 ml, 2.38M) was added. The mixture was stirred at 0° C. for 20 minutes. The ice-bath was replaced by a dry ice-acetone bath and a solution of ethyl benzylidine glycinate (0.445 g) in THF (2 ml) wa...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester.Primary amine
null
null
c1ccc2c(c1)COC2
HBr
CN(C)P(=O)(N(C)C)N(C)C.C1CCOC1
0
0.333333
CCOC(C)=O.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2.[NH4+]>CN(C)P(=O)(N(C)C)N(C)C.C1CCOC1>CCOC(=O)C(N)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-2f7d3cefcf884ad1aca8cee6ff44c882
CCOC(=O)C(N)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2.CS(=O)(=O)Cl>>CCOC(=O)C(C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O)NS(C)(=O)=O
COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)N)\C)OC)C)=O.C(C)N(CC)CC.CS(=O)(=O)Cl>>OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)NS(=O)(=O)C)\C)OC)C)=O
COCCOC[O:14][c:13]1[c:12]([CH2:11]/[CH:10]=[C:8](/[CH2:7][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[NH2:26])[CH3:9])[c:19]([O:20][CH3:21])[c:17]([CH3:18])[c:16]2[c:15]1[C:24](=[O:25])[O:23][CH2:22]2.Cl[S:27]([CH3:28])(=[O:29])=[O:30]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7]/[C:8]([CH3:9])=[CH:10]/[CH2:11][c:12]1[c...
CCOC(=O)C(N)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2.CS(=O)(=O)Cl
CCOC(=O)C(C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O)NS(C)(=O)=O
null
null
C(Cl)Cl
Acylation
OtherReaction
f64aef4580e1e6ad92b3d71ef18da39eb289cd14c0135adab56405f63c8662ac
d8b7bf55ed6b85f502ad9039ef600b9b0dfa1f31935b329cea56a7ab8526271d
O=C1OCc2ccccc21
C-O-C-C-O-C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](=[O;D1;H0:6])-[#8:7].[C:8]=[C:9]/[C:10]-[C:11](-[NH2;D1;+0:12])-[C:13](=[O;D1;H0:14])-[#8:15]-[C:16].Cl-[S;H0;D4;+0:17](-[C;D1;H3:18])(=[O;D1;H0:19])=[O;D1;H0:20]>>[#8:7]-[C:5](=[O;D1;H0:6])-[c:4]:[c:2](-[OH;D1;+0:1]):[c:3].[C:8]=[C:9]/[C:10]-[C:11](-[NH;D2;+0:12]-[S...
82
[{"value": 82.0, "product": "OC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)NS(=O)(=O)C)\\C)OC)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
2
HOUR
Ethyl (E)-6-(4-methoxyethoxymethoxy-1,3-dihydro-6-methoxy-7-methyl -3-oxoisobenzofuran-5-yl)-2-amino-4-methyl-4-hexenoate (373 mg) was dissolved in CH2Cl2 (10 ml), cooled to 0° C., and triethylamine (0.17 ml) and methylsulfonyl chloride (0.09 ml) were added. The mixture was stirred at 0° C. for 1 hour and at room tempe...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Primary amine.Sulfonyl halide
Sulfonamide.Aromatic alcohol
null
null
c1ccc2c(c1)COC2
HCl
C(Cl)Cl
0
2
CCOC(=O)C(N)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2.CS(=O)(=O)Cl>C(Cl)Cl>CCOC(=O)C(C/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O)NS(C)(=O)=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-8e444441d4214018adf3d389f94b601f
CCOC(=O)C(C)C.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2>>CCOC(=O)C(C)(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
[NH4+].[Cl-].C(C)(C)[N-]C(C)C.[Li+].C(C(C)C)(=O)OCC.COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CBr)\C>>COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)(C)C)\C)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH3:7])[CH3:8].Br[CH2:9]/[C:10]([CH3:11])=[CH:12]/[CH2:13][c:14]1[c:15]([O:16][CH3:17])[c:18]([CH3:19])[c:20]2[c:21]([c:22]1[O:23][CH2:24][O:25][CH2:26][CH2:27][O:28][CH3:29])[C:30](=[O:31])[O:32][CH2:33]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[CH2:9]/[C:10]([CH...
CCOC(=O)C(C)C.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2
CCOC(=O)C(C)(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
null
null
CN(C)P(=O)(N(C)C)N(C)C.C(Cl)Cl.CCOC(=O)C.C1CCOC1
C-C Coupling
OtherReaction
cce1a125a1ff1ac49e6bca841c71f39abbf2c962f7edb2747b8c98f3307cb502
0061a06af9fc64155952582b91b574e4abd8908ca14244f15179c2400b24dd08
O=C1OCc2ccccc21
Br-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[C;D1;H3:12])-[C;D1;H3:13]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[C;H0;D4;+0:11](-[C;D1;H3:12])(-[C;D1;H3:13])-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6]
74
[{"value": 74.0, "product": "COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)(C)C)\\C)OC)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
-78
CELSIUS
40
MINUTE
A freshly prepared solution of lithium diisopropylamide (2.8 mmol/10 ml THF) was cooled to -78° C. and ethyl isobutyrate (0.75 ml) was added slowly. The solution was stirred at -78° C. for 40 minutes and then a solution of (E)-4-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy-7-methyl -3-oxoisobenzofuran-5-yl)-2-methylbu...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester
null
null
c1ccc2c(c1)COC2
HBr
CN(C)P(=O)(N(C)C)N(C)C.C(Cl)Cl.CCOC(=O)C.C1CCOC1
-78
0.666667
CCOC(=O)C(C)C.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2>CN(C)P(=O)(N(C)C)N(C)C.C(Cl)Cl.CCOC(=O)C.C1CCOC1>CCOC(=O)C(C)(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-c4e229a8b75d49bea2d79b6f95430408
CCOC(=O)C(C)(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2>>COCCOCOc1c(C/C=C(\C)CC(C)(C)C(=O)O)c(OC)c(C)c2c1C(=O)OC2
COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)(C)C)\C)OC)C)=O>>COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)O)(C)C)\C)OC)C)=O
CC[O:20][C:18]([C:15]([CH2:14]/[C:12](=[CH:11]/[CH2:10][c:9]1[c:8]([O:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])[c:27]2[c:26]([c:24]([CH3:25])[c:21]1[O:22][CH3:23])[CH2:31][O:30][C:28]2=[O:29])[CH3:13])([CH3:16])[CH3:17])=[O:19]>>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][c:8]1[c:9]([CH2:10]/[CH:11]=[C:12](\[CH3:13])[C...
CCOC(=O)C(C)(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2
COCCOCOc1c(C/C=C(\C)CC(C)(C)C(=O)O)c(OC)c(C)c2c1C(=O)OC2
null
null
CCCCCC.C(C)(=O)OCC
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccccc21
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
By following the procedure of Example ZA-6A and substituting methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl) -2,4-dimethyl-4-hexenoate with ethyl (E)-6-(4-methoxyethoxymethoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2,2,4-trimethyl -4-hexenoate and compounds of Formula 10...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccc2c(c1)COC2
Other
CCCCCC.C(C)(=O)OCC
null
null
CCOC(=O)C(C)(C)C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2>CCCCCC.C(C)(=O)OCC>COCCOCOc1c(C/C=C(\C)CC(C)(C)C(=O)O)c(OC)c(C)c2c1C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-6b852ad794654a8dae8183b02d827428
CCOC(=O)CP(=O)(OC)OC.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2>>CCOC(=O)C(C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2)P(=O)(OC)OC
COC1=C(C(=C2C(OCC2=C1C)=O)OCOCCOC)C/C=C(/CBr)\C.COP(=O)(OC)CC(=O)OCC.[H-].[Na+]>>COCCOCOC1=C2C(OCC2=C(C(=C1C/C=C(/CC(C(=O)OCC)P(=O)(OC)OC)\C)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][P:32](=[O:33])([O:34][CH3:35])[O:36][CH3:37].Br[CH2:7]/[C:8]([CH3:9])=[CH:10]/[CH2:11][c:12]1[c:13]([O:14][CH3:15])[c:16]([CH3:17])[c:18]2[c:19]([c:20]1[O:21][CH2:22][O:23][CH2:24][CH2:25][O:26][CH3:27])[C:28](=[O:29])[O:30][CH2:31]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7...
CCOC(=O)CP(=O)(OC)OC.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2
CCOC(=O)C(C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2)P(=O)(OC)OC
null
null
CN(C)C=O
C-C Coupling
OtherReaction
cce1a125a1ff1ac49e6bca841c71f39abbf2c962f7edb2747b8c98f3307cb502
0061a06af9fc64155952582b91b574e4abd8908ca14244f15179c2400b24dd08
O=C1OCc2ccccc21
Br-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6].[#8:7]-[#15:8](-[#8:9])(=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[#8:7]-[#15:8](-[#8:9])(=[O;D1;H0:10])-[CH;D3;+0:11](-[CH2;D2;+0:1]/[C:2](-[C;D1;H3:3])=[C:4]/[C:5]-[c:6])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
null
[]
null
null
10
MINUTE
To a solution of ethyl dimethylphosphonoacetate (135 mg) in DMF (5 ml) at 0° was added 50% NaH/oil (33 mg), and the mixture stirred for 10 minutes. (E)-4-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy7-methyl -3-oxoisobenzofuran-5-yl)-2-methylbut-2-enyl bromide (600 mg) was added at the same temperature and allowed to r...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester
Ester
null
null
c1ccc2c(c1)COC2
HBr
CN(C)C=O
null
0.166667
CCOC(=O)CP(=O)(OC)OC.COCCOCOc1c(C/C=C(\C)CBr)c(OC)c(C)c2c1C(=O)OC2>CN(C)C=O>CCOC(=O)C(C/C(C)=C/Cc1c(OC)c(C)c2c(c1OCOCCOC)C(=O)OC2)P(=O)(OC)OC
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d3b13ccbffa14eb7a6ef6bc77b1e81ca
COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)C(=O)OC(C)(C)C)C(=O)OC2>>COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)C(=O)O)C(=O)OC2
CS(=O)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C(\C(=O)OC(C)(C)C)/Cl)OC)C)=O>>CS(=O)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C(\C(=O)O)/Cl)OC)C)=O
CC(C)(C)[O:21][C:19](/[C:17](=[CH:16]\[CH2:15][c:14]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[O:9][S:10]([CH3:11])(=[O:12])=[O:13])[C:22](=[O:23])[O:24][CH2:25]2)[Cl:18])=[O:20]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10]([CH3:11])(=[O:12])=[O:13])[c:14]1[CH2:15]/[CH:16]=[C:17](/[Cl:18])[C...
COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)C(=O)OC(C)(C)C)C(=O)OC2
COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)C(=O)O)C(=O)OC2
null
null
C(Cl)Cl.FC(C(=O)O)(F)F
Deprotection
Deprotection of carboxylic acid
152e5537e48c95b4a3e767536b0f9f68d1308e5f484070828ab5ed951805157a
7f019d4cfe9b3036d0a2d3a3209aa0e1fcb05418ebee15a4be5e125d315d5f01
O=C1OCc2ccccc21
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])/[C:4](-[Cl;D1;H0:5])=[C:6]\[C:7]>>[C:7]/[C:6]=[C:4](/[Cl;D1;H0:5])-[C:2](=[O;D1;H0:3])-[OH;D1;+0:1]
89.4
[{"value": 89.4, "product": "CS(=O)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C(\\C(=O)O)/Cl)OC)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
90
MINUTE
t-Butyl (E)-4-(1,3-dihydro-4-methanesulfonyloxy-6-methoxy-7-methyl -3-oxoisobenzofuran-5-yl)-2-chlorobut-2-enoate (2.7 g) was dissolved in freshly distilled trifluoroacetic acid (25 ml) and stirred at room temperature for 90 minutes. The mixture was diluted with CH2Cl2 (25 ml) and evaporated to dryness and repeated unt...
10.6084/m9.figshare.5104873.v1
null
Ester.Boc
Carboxylic acid
null
null
c1ccc2c(c1)COC2
Other
C(Cl)Cl.FC(C(=O)O)(F)F
null
1.5
COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)C(=O)OC(C)(C)C)C(=O)OC2>C(Cl)Cl.FC(C(=O)O)(F)F>COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)C(=O)O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-345a467f4df54eeeb4868c55d548a875
CCOC(=O)CC(=O)OCC.COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)CBr)C(=O)OC2>>CCOC(=O)C(C/C(Cl)=C\Cc1c(OC)c(C)c2c(c1OS(C)(=O)=O)C(=O)OC2)C(=O)OCC
CS(=O)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C(\CBr)/Cl)OC)C)=O.C(CC(=O)OCC)(=O)OCC.[H-].[Na+]>>CS(=O)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C(\CC(C(=O)OCC)C(=O)OCC)/Cl)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C:30](=[O:31])[O:32][CH2:33][CH3:34].Br[CH2:7]/[C:8]([Cl:9])=[CH:10]\[CH2:11][c:12]1[c:13]([O:14][CH3:15])[c:16]([CH3:17])[c:18]2[c:19]([c:20]1[O:21][S:22]([CH3:23])(=[O:24])=[O:25])[C:26](=[O:27])[O:28][CH2:29]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7]/[C:8]([Cl:9])=[CH:1...
CCOC(=O)CC(=O)OCC.COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)CBr)C(=O)OC2
CCOC(=O)C(C/C(Cl)=C\Cc1c(OC)c(C)c2c(c1OS(C)(=O)=O)C(=O)OC2)C(=O)OCC
null
null
C1CCOC1
C-C Coupling
OtherReaction
8175b6573d6439ec7ccc45bf6b48843ab56b46dccfc6504384c4766d09f35cc7
d1817e44576d3a158547867a56245217a593d4f828a6d6dfaa8ed11276894e44
O=C1OCc2ccccc21
Br-[CH2;D2;+0:1]/[C:2](-[Cl;D1;H0:3])=[C:4]\[C:5]-[c:6].[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH2;D2;+0:11]-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]>>[C:7]-[#8:8]-[C:9](=[O;D1;H0:10])-[CH;D3;+0:11](-[CH2;D2;+0:1]/[C:2](-[Cl;D1;H0:3])=[C:4]\[C:5]-[c:6])-[C:12](=[O;D1;H0:13])-[#8:14]-[C:15]
57.5
[{"value": 57.5, "product": "CS(=O)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C(\\CC(C(=O)OCC)C(=O)OCC)/Cl)OC)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
Diethyl malonate (113 mg) was added to a suspension of 50% NaH (35 mg) in THF (3 ml) at 0° C. and the mixture stirred for 30 minutes. To this solution was added (E)-4-(1,3-dihydro-4-methanesulfonyloxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-1-bromo-2-chlorobut-2-ene (280 mg) in THF (10 ml). The ice bath was removed...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ester
Ester.Ester
null
null
c1ccc2c(c1)COC2
HBr
C1CCOC1
null
0.5
CCOC(=O)CC(=O)OCC.COc1c(C)c2c(c(OS(C)(=O)=O)c1C/C=C(/Cl)CBr)C(=O)OC2>C1CCOC1>CCOC(=O)C(C/C(Cl)=C\Cc1c(OC)c(C)c2c(c1OS(C)(=O)=O)C(=O)OC2)C(=O)OCC
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a0f89bc489b2437c8013eb1e5e984063
C=C(C)C(O)Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.COC(CCCBr)(OC)OC>>COC(=O)C(CCBr)CC(C)=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
C(CC)(=O)O.[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1CC(C(=C)C)O)OC)C)=O.COC(CCCBr)(OC)OC>>BrCCC(C(=O)OC)CC(=CCC=1C(=C2C(OCC2=C(C1OC)C)=O)O[Si](C)(C)C(C)(C)C)C
O[CH:12]([C:10](=[CH2:9])[CH3:11])[CH2:13][c:14]1[c:15]([O:16][CH3:17])[c:18]([CH3:19])[c:20]2[c:21]([c:22]1[O:23][Si:24]([CH3:25])([CH3:26])[C:27]([CH3:28])([CH3:29])[CH3:30])[C:31](=[O:32])[O:33][CH2:34]2.CO[C:3]([O:2][CH3:1])([O:4]C)[CH2:5][CH2:6][CH2:7][Br:8]>>[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][CH2:7][Br:8])[C...
C=C(C)C(O)Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.COC(CCCBr)(OC)OC
COC(=O)C(CCBr)CC(C)=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
null
null
Acylation
OtherReaction
9bf7c01f3fba65ea0cdc8ffe3c902a1716bf21528f214415a6c56fa7fdc4a193
c738d9923191e0b9d66534a280f828a4b3af1448c6f50b64792c7c450a24abfc
O=C1OCc2ccccc21
C-O-[C;H0;D4;+0:1](-[#8:2]-[C;D1;H3:3])(-[CH2;D2;+0:4]-[C:5]-[C:6])-[O;H0;D2;+0:7]-C.O-[CH;D3;+0:8](-[C:9]-[c:10])-[C;H0;D3;+0:11](-[C;D1;H3:12])=[CH2;D1;+0:13]>>[C:6]-[C:5]-[CH;D3;+0:4](-[CH2;D2;+0:13]-[C;H0;D3;+0:11](-[C;D1;H3:12])=[CH;D2;+0:8]-[C:9]-[c:10])-[C;H0;D3;+0:1](=[O;H0;D1;+0:7])-[#8:2]-[C;D1;H3:3]
null
[]
null
null
null
null
A solution of trimethyl 4-bromoorthobutyrate (20 ml), propionic acid (0.22 ml) and 4-(4-tert-butyldimethylsilyloxy-1,3-dihydro-6-methoxy -7-methyl-3-oxoisobenzofuran-5-yl)-3-hydroxy-2-methylbut-1-ene (3.18 g) was heated at 110° C. in a three-necked flash with a slow nitrogen stream passing over the reaction mixture. Af...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Ether.Secondary alcohol.Vinyl
Ester
null
null
c1ccc2c(c1)COC2
HO-
null
null
null
C=C(C)C(O)Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.COC(CCCBr)(OC)OC>>COC(=O)C(CCBr)CC(C)=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0ae8071f8fc94140b0001a99db3d857b
CC(C)NC(C)C.COC(=O)C(CCBr)CC(C)=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>CC(C)[N-]C(C)C.COC(=O)C1(CC(C)=CCc2c(OC)c(C)c3c(c2O[Si](C)(C)C(C)(C)C)C(=O)OC3)CC1
C(C)(C)NC(C)C.C(CCC)[Li].BrCCC(C(=O)OC)CC(=CCC=1C(=C2C(OCC2=C(C1OC)C)=O)O[Si](C)(C)C(C)(C)C)C.[Li+].CC(C)[N-]C(C)C>>C(C)(C)[N-]C(C)C.[Li+].COC(=O)C1(CC1)CC(=CCC=1C(=C2C(OCC2=C(C1OC)C)=O)O[Si](C)(C)C(C)(C)C)C
[CH3:1][CH:2]([CH3:3])[NH:4][CH:5]([CH3:6])[CH3:7].Br[CH2:40][CH2:39][CH:12]([C:10]([O:9][CH3:8])=[O:11])[CH2:13][C:14]([CH3:15])=[CH:16][CH2:17][c:18]1[c:19]([O:20][CH3:21])[c:22]([CH3:23])[c:24]2[c:25]([c:26]1[O:27][Si:28]([CH3:29])([CH3:30])[C:31]([CH3:32])([CH3:33])[CH3:34])[C:35](=[O:36])[O:37][CH2:38]2>>[CH3:1][C...
CC(C)NC(C)C.COC(=O)C(CCBr)CC(C)=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
CC(C)[N-]C(C)C.COC(=O)C1(CC(C)=CCc2c(OC)c(C)c3c(c2O[Si](C)(C)C(C)(C)C)C(=O)OC3)CC1
null
null
C1CCOC1
C-C Coupling
OtherReaction
954c2f92326cf05ea81d7d009ca43bf34835471a23144b5f5879cbf4cbe25ec0
6e06776731664fe9861b643a9b8e2db1cb60f0e675c8f3b0a8d851226bbe26c6
O=C1OCc2ccc(CC=CCC3CC3)cc21
Br-[CH2;D2;+0:1]-[C:2]-[CH;D3;+0:3](-[C:4]-[C:5](-[C;D1;H3:6])=[C:7]-[C:8])-[C:9](=[O;D1;H0:10])-[#8:11]-[C;D1;H3:12].[C;D1;H3:13]-[C:14](-[C;D1;H3:15])-[NH;D2;+0:16]-[C:17](-[C;D1;H3:18])-[C;D1;H3:19]>>[C;D1;H3:13]-[C:14](-[C;D1;H3:15])-[N-;H0;D2:16]-[C:17](-[C;D1;H3:18])-[C;D1;H3:19].[C:8]-[C:7]=[C:5](-[C;D1;H3:6])-[...
null
[]
-70
CELSIUS
50
MINUTE
A solution of lithium diisopropyl amide was prepared from diisopropyl amine (2.24 ml) and n-butyllithium (6.4 ml, 2.5N) in THF (60 ml) and cooled to -70° C. Methyl 2-(2-bromoethyl)-6-(4-t-butyldimethylsiloxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran -5-yl)-4-methyl-hex-4-enoate (2.66 g) in THF (12 ml was added ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Secondary amine
Ester
null
C1CC1
c1ccc2c(c1)COC2.C1CC1
HBr
C1CCOC1
-70
0.833333
CC(C)NC(C)C.COC(=O)C(CCBr)CC(C)=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>C1CCOC1>CC(C)[N-]C(C)C.COC(=O)C1(CC(C)=CCc2c(OC)c(C)c3c(c2O[Si](C)(C)C(C)(C)C)C(=O)OC3)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d4d6d955703f412fbc9575b9b91423d7
COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)O)C(=O)OC2.O=S(Cl)Cl>>COc1c(C)c2c(c(O)c1CC=C(C)CCC(=O)Cl)C(=O)OC2
CC1=C2C(=C(C(=C1OC)C/C=C(\C)/CCC(=O)O)O)C(=O)OC2.CN(C=O)C.S(=O)(Cl)Cl>>OC1=C2C(OCC2=C(C(=C1CC=C(CCC(=O)Cl)C)OC)C)=O
O[C:17]([CH2:16][CH2:15]/[C:13](=[CH:12]/[CH2:11][c:10]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[OH:9])[C:20](=[O:21])[O:22][CH2:23]2)[CH3:14])=[O:18].O=S(Cl)[Cl:19]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11][CH:12]=[C:13]([CH3:14])[CH2:15][CH2:16][C:17](=[O:18])[Cl:19])[C:20](...
COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)O)C(=O)OC2.O=S(Cl)Cl
COc1c(C)c2c(c(O)c1CC=C(C)CCC(=O)Cl)C(=O)OC2
null
null
ClCCl
Functional Group Interconversion
Alcohol to chloride_SOCl2
c301c14a9dcd0670d52e8b77396cbe7fd8edeedd757bc43f4162ade1fc52fc93
787f545db5dc0b29dde55b5fbed7db8625b8055f49327f97ed4d83cc47c3af1d
O=C1OCc2ccccc21
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[C:4]-[C:5]\[C:6]=[C:7]>>[C:7]=[C:6]-[C:5]-[C:4]-[C;H0;D3;+0:2](-[Cl;H0;D1;+0:1])=[O;D1;H0:3]
null
[]
null
null
null
null
A solution of mycophenolic acid (320 g, 1 mol) and dimethylformamide (0.1 g) in dichloromethane (3.2L) at reflux was treated dropwise with thionyl chloride (82 mL, 1.12 mol). After one hour additional heating at reflux, the volatiles were distilled at reduced pressure leaving a gray solid residue of (E) 6-(1,3-dihydro-...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Acyl halide
null
null
c1ccc2c(c1)COC2
HCl
ClCCl
null
null
COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)O)C(=O)OC2.O=S(Cl)Cl>ClCCl>COc1c(C)c2c(c(O)c1CC=C(C)CCC(=O)Cl)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d10d3d4f2cce4f3e823df84d28be081a
COc1c(C)c2c(c(O)c1CC=C(C)CCC(=O)Cl)C(=O)OC2.O=C1N[C@@H](Cc2ccccc2)CO1>>COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2
Cl.OC1=C2C(OCC2=C(C(=C1CC=C(CCC(=O)Cl)C)OC)C)=O.C(CCC)[Li].CCCCCC.C(C1=CC=CC=C1)[C@@H]1NC(OC1)=O.C(C)(C)(C)O>>C(C1=CC=CC=C1)C1N(C(OC1)=O)C(CC\C(=C\CC=1C(=C2C(OCC2=C(C1OC)C)=O)O)\C)=O
Cl[C:17]([CH2:16][CH2:15][C:13](=[CH:12][CH2:11][c:10]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[OH:9])[C:32](=[O:33])[O:34][CH2:35]2)[CH3:14])=[O:18].[NH:19]1[C:20](=[O:21])[O:22][CH2:23][C@@H:24]1[CH2:25][c:26]1[cH:27][cH:28][cH:29][cH:30][cH:31]1>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c...
COc1c(C)c2c(c(O)c1CC=C(C)CCC(=O)Cl)C(=O)OC2.O=C1N[C@@H](Cc2ccccc2)CO1
COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2
null
null
O1CCCC1.C(C)(=O)OCC
Protection
N-alkylation of secondary amines with alkyl halides
90b874b95a490ba678a8102349b0a4dbcd41213027fb4e6cf3a650d8fd23bd0d
4e5209ce9341ab4af6dffbdfa22c50d4dc790b976013dec4e496751ff4457c48
O=C1OCc2ccc(CC=CCCC(=O)N3C(=O)OCC3Cc3ccccc3)cc21
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4]-[C:5]=[C:6].[O;D1;H0:7]=[C:8]1-[#8:9]-[C:10]-[C@H;D3;+0:11](-[C:12]-[c:13])-[NH;D2;+0:14]-1>>[C:6]=[C:5]/[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[N;H0;D3;+0:14]1-[C:8](=[O;D1;H0:7])-[#8:9]-[C:10]-[CH;D3;+0:11]-1-[C:12]-[c:13]
null
[]
0
CELSIUS
null
null
A solution of (S)-4-benzyl-2-oxazolidinone (177.4 g, 1 mol) and t-butyl alcohol (74.1 g , 1 mol) in anhydrous tetrahydrofuran (2L) was cooled to -78° C. A 1.6M solution of n-butyllithium in hexane (1280 mL, 2 mol) was added maintaining a temperature below -30° C. After recooling to -78° C. the (E) 6-(1,3-dihydro-4-hydr...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Carbamic ester
Carbamic ester.Substituted dicarboximide
C1COCN1
C1COC[NH]1
C1COC[NH]1.c1ccccc1.c1ccc2c(c1)COC2
HCl
O1CCCC1.C(C)(=O)OCC
0
null
COc1c(C)c2c(c(O)c1CC=C(C)CCC(=O)Cl)C(=O)OC2.O=C1N[C@@H](Cc2ccccc2)CO1>O1CCCC1.C(C)(=O)OCC>COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a76e7895a60a43e49f3e09dc222840eb
CI.COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2.C[Si](C)(C)[N-][Si](C)(C)C>>COc1c(C)c2c(c(O)c1C/C=C(\C)CC(C)C(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2.COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2
Cl.C(C1=CC=CC=C1)C1N(C(OC1)=O)C(CC\C(=C\CC=1C(=C2C(OCC2=C(C1OC)C)=O)O)\C)=O.IC.C[Si](C)(C)[N-][Si](C)(C)C.[Na+]>>C(C1=CC=CC=C1)C1N(C(OC1)=O)C(CC\C(=C\CC=1C(=C2C(OCC2=C(C1OC)C)=O)O)\C)=O.C(C1=CC=CC=C1)C1N(C(OC1)=O)C(C(C\C(=C\CC=1C(=C2C(OCC2=C(C1OC)C)=O)O)\C)C)=O
I[CH3:17].[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:47]/[CH:48]=[C:49](\[CH3:50])[CH2:51][CH2:52][C:53](=[O:54])[N:55]1[C:56](=[O:57])[O:58][CH2:59][CH:60]1[CH2:61][c:62]1[cH:63][cH:64][cH:65][cH:66][cH:67]1)[C:68](=[O:69])[O:70][CH2:71]2.[Si]([CH3:11])([N-:20][Si]([CH3:24])([CH3:26])[CH3:42]...
CI.COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2.C[Si](C)(C)[N-][Si](C)(C)C
COc1c(C)c2c(c(O)c1C/C=C(\C)CC(C)C(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2.COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2
null
null
O1CCCC1
Aromatic Heterocycle Formation
OtherReaction
c3747f16c99e5a8882af06091809359bc45494249716c48d4f2edbc76532e2aa
6086e6621f5fe9e2ec64c99724be0620d1ebc7e7a8ff5acda211b311ca7cf66b
O=C1OCc2ccc(CC=CCCC(=O)N3C(=O)OCC3Cc3ccccc3)cc21.O=C1OCc2ccc(CC=CCCC(=O)N3C(=O)OCC3Cc3ccccc3)cc21
I-[CH3;D1;+0:1].[#7:2]-[C:3](=[O;D1;H0:4])-[C:5]-[C:6]/[C:7](-[C;D1;H3:8])=[C:9]/[CH2;D2;+0:10]-[c;H0;D3;+0:11]1:[c:12](-[#8:13]):[c:14](-[C;D1;H3:15]):[c;H0;D3;+0:16]2:[c;H0;D3;+0:17](:[c:18]:1-[O;D1;H1:19])-[C;H0;D3;+0:20](=[O;D1;H0:21])-[#8:22]-[CH2;D2;+0:23]-2.[CH3;D1;+0:24]-[Si](-[CH3;D1;+0:25])(-[CH3;D1;+0:26])-[...
null
[]
-30
CELSIUS
15
MINUTE
A 1M solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran (0.43L, 0.43 mol) was cooled to -78° C. and treated dropwise with a precooled solution of (S) 4-benzyl-3-[(E) 6-(1,3-dihydro-4-hydroxy -6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-4-methyl-4-hexenoyl]-2-oxazolidinone (86 g, 0.179 mol) in tetrahydrofura...
10.6084/m9.figshare.5104873.v1
null
Ester.Silyl protective group.Silyl protective group
Carbamic ester.Ester.Ester.Ether.Ether.Substituted dicarboximide.Aromatic alcohol
c1ccc2c(c1)COC2
C1COC[NH]1.c1ccccc1.c1ccc2c(c1)COC2.c1ccc2c(c1)COC2
C1COC[NH]1.c1ccccc1.c1ccc2c(c1)COC2.C1COC[NH]1.c1ccccc1.c1ccc2c(c1)COC2
I-
O1CCCC1
-30
0.25
CI.COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2.C[Si](C)(C)[N-][Si](C)(C)C>O1CCCC1>COc1c(C)c2c(c(O)c1C/C=C(\C)CC(C)C(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2.COc1c(C)c2c(c(O)c1C/C=C(\C)CCC(=O)N1C(=O)OCC1Cc1ccccc1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3c98506f7b5947428a6899a4897143df
COc1c(C)c2c(c(O)c1CC=C(C)CC(C)C(=O)O)C(=O)OC2>>COc1c(C)c2c(c(O)c1CC=C(C)CC(C)C(=O)O)C(=O)OC2
OC1=C2C(OCC2=C(C(=C1CC=C(CC(C(=O)O)C)C)OC)C)=O.CC(C1=CC=CC=C1)N>>CC(C1=CC=CC=C1)N.OC1=C2C(OCC2=C(C(=C1CC=C(CC(C(=O)O)C)C)OC)C)=O
[CH3:10][O:11][c:12]1[c:13]([CH3:14])[c:15]2[c:16]([c:17]([OH:18])[c:19]1[CH2:20][CH:21]=[C:22]([CH3:23])[CH2:24][CH:25]([CH3:26])[C:27](=[O:28])[OH:29])[C:30](=[O:31])[O:32][CH2:33]2>>[CH3:10][O:11][c:12]1[c:13]([CH3:14])[c:15]2[c:16]([c:17]([OH:18])[c:19]1[CH2:20][CH:21]=[C:22]([CH3:23])[CH2:24][CH:25]([CH3:26])[C:27...
COc1c(C)c2c(c(O)c1CC=C(C)CC(C)C(=O)O)C(=O)OC2
COc1c(C)c2c(c(O)c1CC=C(C)CC(C)C(=O)O)C(=O)OC2
null
null
CC(=O)C
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
O=C1OCc2ccccc21
null
null
[]
null
null
null
null
A solution of the 85:13 acid mixture(E) 6-(1,3-dihydro-4-hydroxy -6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2,4-dimethyl-4-hexenoic acid (810 g, 2.4 mol,) was dissolved in acetone (16L) at 40° C. and (+)-α-methylbenzylamine (800 g, 6.6 mol) was added. Upon cooling, the salt crystallized and was collected by filtratio...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccc2c(c1)COC2
null
CC(=O)C
null
null
COc1c(C)c2c(c(O)c1CC=C(C)CC(C)C(=O)O)C(=O)OC2>CC(=O)C>COc1c(C)c2c(c(O)c1CC=C(C)CC(C)C(=O)O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a413010b44c54d4998306c0743d3f4dd
COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)C1=CCCC1)C(=O)OC2>>COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(=O)C1=CCCC1)C(=O)OC2
C(C)N(CC)CC.[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1CC(O)C1=CCCC1)OC)C)=O.FC(C(=O)OC(C(F)(F)F)=O)(F)F.CS(=O)C>>C1(=CCCC1)C(=O)CC=1C(=C2C(OCC2=C(C1OC)C)=O)O[Si](C)(C)C(C)(C)C
[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][Si:10]([CH3:11])([CH3:12])[C:13]([CH3:14])([CH3:15])[CH3:16])[c:17]1[CH2:18][CH:19]([OH:20])[C:21]1=[CH:22][CH2:23][CH2:24][CH2:25]1)[C:26](=[O:27])[O:28][CH2:29]2>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][Si:10]([CH3:11])([CH3:12])[C:13]([CH3:14])(...
COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)C1=CCCC1)C(=O)OC2
COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(=O)C1=CCCC1)C(=O)OC2
null
null
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C(Cc1ccc2c(c1)C(=O)OC2)C1=CCCC1
[C:1]-[C:2]=[C:3](-[CH;D3;+0:4](-[OH;D1;+0:5])-[C:6]-[c:7])-[C:8]>>[C:1]-[C:2]=[C:3](-[C;H0;D3;+0:4](=[O;H0;D1;+0:5])-[C:6]-[c:7])-[C:8]
82.9
[{"value": 82.9, "product": "C1(=CCCC1)C(=O)CC=1C(=C2C(OCC2=C(C1OC)C)=O)O[Si](C)(C)C(C)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-40
CELSIUS
30
MINUTE
Trifluoroacetic anhydride (1.6 ml) in methylene chloride (3.6 ml) was added dropwise to dimethyl sulfoxide (1.05 ml) and CH2Cl2 (7.5 ml) under nitrogen over 5 minutes at -60° C. and stirred for 30 minutes. After addition of (±)-2-(4-tert-butyldimethylsilyloxy-1,3-dihydro-6-methoxy -7-methyl-3-oxoisobenzofuran-5-yl)-1-c...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
C1=CCCC1.c1ccc2c(c1)COC2
null
C(Cl)Cl
-40
0.5
COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)C1=CCCC1)C(=O)OC2>C(Cl)Cl>COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(=O)C1=CCCC1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0b6617e9cfd7449aaea81f512395c478
CC(C)(C)C(=O)O.CCC(CC)(CC)C([O-])([O-])[O-].COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)C1=CCCC1)C(=O)OC2>>CCOC(=O)CC1CCC/C1=C\Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1CC(O)C1=CCCC1)OC)C)=O.C(C(C)(C)C)(=O)O.C(C)C(C([O-])([O-])[O-])(CC)CC>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C\C=C/1\C(CCC1)CC(=O)OCC)OC)C)=O
C[C:6](C)(C)[C:4]([OH:3])=[O:5].CCC(CC)(C([O-])([O-])[O-])[CH2:2][CH3:1].O[CH:12]([C:11]1=[CH:7][CH2:8][CH2:9][CH2:10]1)[CH2:13][c:14]1[c:15]([O:16][CH3:17])[c:18]([CH3:19])[c:20]2[c:21]([c:22]1[O:23][Si:24]([CH3:25])([CH3:26])[C:27]([CH3:28])([CH3:29])[CH3:30])[C:31](=[O:32])[O:33][CH2:34]2>>[CH3:1][CH2:2][O:3][C:4](=...
CC(C)(C)C(=O)O.CCC(CC)(CC)C([O-])([O-])[O-].COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)C1=CCCC1)C(=O)OC2
CCOC(=O)CC1CCC/C1=C\Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
null
C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
edea5afb4f08e3f70490ee1fcf435c71451d86fc16b124dbfe27b4c4de1bc2d7
505f7b4da8def84a80ac616845cb7b0566b14f3232b5b9d3480d84d3e0d284a0
O=C1OCc2ccc(CC=C3CCCC3)cc21
C-C-C(-C-C)(-[CH2;D2;+0:1]-[C;D1;H3:2])-C(-[O-])(-[O-])-[O-].C-[C;H0;D4;+0:3](-C)(-C)-[C:4](=[O;D1;H0:5])-[OH;D1;+0:6].O-[CH;D3;+0:7](-[C:8]-[c:9])-[C;H0;D3;+0:10]1=[CH;D2;+0:11]-[C:12]-[C:13]-[C:14]-1>>[C;D1;H3:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[C:4](=[O;D1;H0:5])-[CH2;D2;+0:3]-[CH;D3;+0:11]1-[C:12]-[C:13]-[C:14]/[C;H0;...
null
[]
100
CELSIUS
null
null
A solution of 1-[2-(4-tert-butyldimethylsilyloxy-1,3-dihydro -6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-1-hydroxyeth-1-yl]cyclopent-1-ene (0.22 g) in triethylorthoacetate (10 ml) was treated with pivalic acid (0.010 g) and then heated to 100° C., and maintained at that temperature for 18 hours. After cooling to ambie...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol
Ester
C1=CCCC1
C1CCCC1
C1CCCC1.c1ccc2c(c1)COC2
HO-
C(C)(=O)OCC
100
null
CC(C)(C)C(=O)O.CCC(CC)(CC)C([O-])([O-])[O-].COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)C1=CCCC1)C(=O)OC2>C(C)(=O)OCC>CCOC(=O)CC1CCC/C1=C\Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-089ee3ae5afb430eb9502365490c6f0d
CCOC(=O)C[C@@H]1CCC/C1=C\Cc1c(O)c2c(c(C)c1OC)COC2=O.CI>>CCOC(=O)C(C)[C@@H]1CCC/C1=C\Cc1c(O)c2c(c(C)c1OC)COC2=O
[Cl-].[NH4+].C[Si](C)(C)[N-][Si](C)(C)C.[Na+].OC1=C2C(OCC2=C(C(=C1C\C=C/1\[C@@H](CCC1)CC(=O)OCC)OC)C)=O.CI>>OC1=C2C(OCC2=C(C(=C1C\C=C/1\[C@@H](CCC1)C(C(=O)OCC)C)OC)C)=O
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][C@@H:8]1[CH2:9][CH2:10][CH2:11]/[C:12]1=[CH:13]\[CH2:14][c:15]1[c:16]([OH:17])[c:18]2[c:19]([c:20]([CH3:21])[c:22]1[O:23][CH3:24])[CH2:25][O:26][C:27]2=[O:28].I[CH3:7]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH3:7])[C@@H:8]1[CH2:9][CH2:10][CH2:11]/[C:12]1=[CH:13]\[CH2:14][c:15]1...
CCOC(=O)C[C@@H]1CCC/C1=C\Cc1c(O)c2c(c(C)c1OC)COC2=O.CI
CCOC(=O)C(C)[C@@H]1CCC/C1=C\Cc1c(O)c2c(c(C)c1OC)COC2=O
null
null
O1CCCC1.CN1C(N(CCC1)C)=O.C(C)(=O)OCC
C-C Coupling
Methylation with MeI_secondary
4a52ebe9ffae5bdd307b0b4ac6a7069bc533ab8d42293ed2712c32b846010273
49d6f28766066d07dffbcc6f4da77792f6ba67b4de619800bad651525d6fe2e7
O=C1OCc2ccc(CC=C3CCCC3)cc21
I-[CH3;D1;+0:1].[C:2]/[C:3](=[C:4]\[C:5])-[C:6](-[CH2;D2;+0:7]-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11])-[C:12]>>[C:2]/[C:3](=[C:4]\[C:5])-[C:6](-[CH;D3;+0:7](-[CH3;D1;+0:1])-[C:8](=[O;D1;H0:9])-[#8:10]-[C:11])-[C:12]
null
[]
null
null
30
MINUTE
To a solution of 1M sodium bis(trimethylsilyl)amide in tetrahydrofuran (31.7 ml ) and 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (2.74 ml) at -78° C. was added ethyl (E) 2-{2-[2-(1,3-dihydro -4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl) ethylidene]cyclopent -1-(S)-yl}acetate (3.39 g) in tetrahydrofuran...
10.6084/m9.figshare.5104873.v1
null
Ester
Ester
null
null
C1CCCC1.c1ccc2c(c1)COC2
HI
O1CCCC1.CN1C(N(CCC1)C)=O.C(C)(=O)OCC
null
0.5
CCOC(=O)C[C@@H]1CCC/C1=C\Cc1c(O)c2c(c(C)c1OC)COC2=O.CI>O1CCCC1.CN1C(N(CCC1)C)=O.C(C)(=O)OCC>CCOC(=O)C(C)[C@@H]1CCC/C1=C\Cc1c(O)c2c(c(C)c1OC)COC2=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9607c20c20c74c6fbe9c3af9fb2b3115
CCC=O.COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=O)C(=O)OC2>>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=C(C)C=O)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=O.C(CC)=O.C1(=CC=CC=C1)C>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=C(C=O)C
[CH2:23]([CH3:24])[CH:25]=[O:26].O=[CH:22][CH2:21][c:20]1[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]2[c:7]([c:8]1[O:9][S:10](=[O:11])(=[O:12])[c:13]1[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]1)[C:27](=[O:28])[O:29][CH2:30]2>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11])(=[O:12])[c:13]3[cH:14][cH:1...
CCC=O.COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=O)C(=O)OC2
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=C(C)C=O)C(=O)OC2
null
null
null
C-C Coupling
OtherReaction
154f038b7f5648ae5349abff8a924c982177f620bdfb6a2f53d7ca0fce37c68d
3174a51604157c488f07402e36f994f716989b8fc10687ee243713b4cfbdb11a
O=C1OCc2cccc(OS(=O)(=O)c3ccccc3)c21
O=[CH;D2;+0:1]-[C:2]-[c:3].[C;D1;H3:4]-[CH2;D2;+0:5]-[C:6]=[O;D1;H0:7]>>[C;D1;H3:4]-[C;H0;D3;+0:5](-[C:6]=[O;D1;H0:7])=[CH;D2;+0:1]-[C:2]-[c:3]
null
[]
null
null
16
HOUR
A solution of 2-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranyl)acetaldehyde (10.0 g) and 2-triphenylphosphoranylidine propionaldehyde (10.3 g) in toluene (150 mL) was heated under nitrogen atmosphere using an oil bath at 80° C. After allowing the reaction to proceed for 16 hours, the mix...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Aldehyde
Aldehyde
null
null
c1ccccc1.c1ccc2c(c1)COC2
HO-
null
null
16
CCC=O.COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=O)C(=O)OC2>>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=C(C)C=O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-cf23d575e9194b7e8f2f8af78c19eb28
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=C(C)C=O)C(=O)OC2>>C=CC(O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=C(C=O)C.C(=C)[Mg]Br>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=C(C(C=C)O)C
[CH:3](=[O:4])[C:5]([CH3:6])=[CH:7][CH2:8][c:9]1[c:10]([O:11][CH3:12])[c:13]([CH3:14])[c:15]2[c:16]([c:17]1[O:18][S:19](=[O:20])(=[O:21])[c:22]1[cH:23][cH:24][c:25]([CH3:26])[cH:27][cH:28]1)[C:29](=[O:30])[O:31][CH2:32]2>>[CH2:1]=[CH:2][CH:3]([OH:4])[C:5]([CH3:6])=[CH:7][CH2:8][c:9]1[c:10]([O:11][CH3:12])[c:13]([CH3:14...
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=C(C)C=O)C(=O)OC2
C=CC(O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
null
null
O1CCCC1.C(C)(=O)OCC
Miscellaneous
OtherReaction
7c95c9d475b3e4739c4b4bffdb557ccc0332365664dc5f751958e7bb4139acbc
1cfdacde78204b273e664dc0eb50ffc4dc70522ea435514fcadd01e492b9b547
O=C1OCc2cccc(OS(=O)(=O)c3ccccc3)c21
[C:1]-[C:2]=[C:3](-[C;D1;H3:4])-[CH;D2;+0:5]=[O;H0;D1;+0:6]>>[C:1]-[C:2]=[C:3](-[C;D1;H3:4])-[CH;D3;+0:5](-[OH;D1;+0:6])-[C:7]=[C;D1;H2:8]
null
[]
null
null
0.5
HOUR
To a solution of 4-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranyl)2-methylbut-2-enaldehyde (0.90 g) in tetrahydrofuran (40 mL) was added vinylmagnesium bromide (4.5 mL of a 1M solution in tetrahydrofuran). After stirring for 0.5 hours, the reaction was diluted with ethyl acetate and wash...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Secondary alcohol.Vinyl
null
null
c1ccccc1.c1ccc2c(c1)COC2
Other
O1CCCC1.C(C)(=O)OCC
null
0.5
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC=C(C)C=O)C(=O)OC2>O1CCCC1.C(C)(=O)OCC>C=CC(O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-976750afea43480dbde7862b5dd1dd25
C=CC(O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2>>C=CC(=O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=C(C(C=C)O)C.[Cr](=O)(=O)([O-])O[Cr](=O)(=O)[O-].[NH+]1=CC=CC=C1.[NH+]1=CC=CC=C1>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=C(C(C=C)=O)C
[CH2:1]=[CH:2][CH:3]([OH:4])[C:5]([CH3:6])=[CH:7][CH2:8][c:9]1[c:10]([O:11][CH3:12])[c:13]([CH3:14])[c:15]2[c:16]([c:17]1[O:18][S:19](=[O:20])(=[O:21])[c:22]1[cH:23][cH:24][c:25]([CH3:26])[cH:27][cH:28]1)[C:29](=[O:30])[O:31][CH2:32]2>>[CH2:1]=[CH:2][C:3](=[O:4])[C:5]([CH3:6])=[CH:7][CH2:8][c:9]1[c:10]([O:11][CH3:12])[...
C=CC(O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
C=CC(=O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
null
null
C(Cl)Cl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
c7c20d2959ac48847b03cc1265962cf99a8ec8a85900c087dabb30077298c66c
767cfd93f5821ebb9e1e72addd9cb404b20b0c821d246ae6b87a5776b74a455b
O=C1OCc2cccc(OS(=O)(=O)c3ccccc3)c21
[C:1]-[C:2]=[C:3](-[C;D1;H3:4])-[CH;D3;+0:5](-[OH;D1;+0:6])-[C:7]=[C;D1;H2:8]>>[C:1]-[C:2]=[C:3](-[C;D1;H3:4])-[C;H0;D3;+0:5](=[O;H0;D1;+0:6])-[C:7]=[C;D1;H2:8]
null
[]
null
null
3
HOUR
The oil product from Example ZC-1B, 6-(1,3-dihydro-6-methoxy -7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranyl)-3-hydroxy -4-methylhexa-1,4-diene, was dissolved in methylene chloride (20 mL) and 4A molecular sieves (2 g) were added. With vigorous stirring, pyridinium dichromate (2 g) was added and the reaction a...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
Ketone
null
null
c1ccccc1.c1ccc2c(c1)COC2
null
C(Cl)Cl
null
3
C=CC(O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2>C(Cl)Cl>C=CC(=O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9bfcdef938be481b93d518222f755bb0
C=CC(=O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2>>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(=O)CC1)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC=C(C(C=C)=O)C.B(F)(F)F.CCOCC>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)=O)C
[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11])(=[O:12])[c:13]3[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]3)[c:20]1[CH2:21][CH:22]=[C:23]([CH3:24])[C:25](=[O:26])[CH:27]=[CH2:28])[C:29](=[O:30])[O:31][CH2:32]2>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11])(=[O:12])[c:13]...
C=CC(=O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(=O)CC1)C(=O)OC2
null
null
C(Cl)Cl.C(C)(=O)OCC
C-C Coupling
OtherReaction
57106fdf64b8b2da8f414882c67b45f14b6a19fc78b6d73b28d8fd2222e3e4d1
2423fd262a32a267ed5d6ae9baff9668729a2c0a60281fcd676d6597312a598b
O=C1C=C(Cc2ccc3c(c2OS(=O)(=O)c2ccccc2)C(=O)OC3)CC1
[C;D1;H3:1]-[C:2](=[CH;D2;+0:3]-[C:4]-[c:5])-[C:6](=[O;D1;H0:7])-[CH;D2;+0:8]=[CH2;D1;+0:9]>>[C;D1;H3:1]-[C:2]1=[C;H0;D3;+0:3](-[C:4]-[c:5])-[CH2;D2;+0:9]-[CH2;D2;+0:8]-[C:6]-1=[O;D1;H0:7]
null
[]
null
null
0.5
HOUR
The solid product prepared in Example ZC-1C, 6-(1,3-dihydro -6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranyl) -4-methylhexa-1,4-dien-3-one was dissolved in methylene chloride (15 mL) and treated with boron trifluoride etherate (0.5 mL). After 0.5 hours, the reaction was diluted with ethyl acetate and ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Vinyl
Ketone
null
C1=CCCC1
c1ccccc1.C1=CCCC1.c1ccc2c(c1)COC2
null
C(Cl)Cl.C(C)(=O)OCC
null
0.5
C=CC(=O)C(C)=CCc1c(OC)c(C)c2c(c1OS(=O)(=O)c1ccc(C)cc1)C(=O)OC2>C(Cl)Cl.C(C)(=O)OCC>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(=O)CC1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a6c7fd2f95eb41c2a437b2e2f311beb5
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(=O)CC1)C(=O)OC2>>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(O)CC1)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)=O)C.O.O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Ce+3].[BH4-].[Na+]>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)O)C
[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11])(=[O:12])[c:13]3[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]3)[c:20]1[CH2:21][C:22]1=[C:23]([CH3:24])[C:25](=[O:26])[CH2:27][CH2:28]1)[C:29](=[O:30])[O:31][CH2:32]2>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11])(=[O:12])[c:13...
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(=O)CC1)C(=O)OC2
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(O)CC1)C(=O)OC2
null
null
O1CCCC1.CO.C(C)(=O)OCC
Reduction
Reduction of ketone to secondary alcohol
cdb715078de81de44f7378b33188a9fd6e2a8cc99d338ab2c91bd5935d725bcf
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
O=C1OCc2ccc(CC3=CCCC3)c(OS(=O)(=O)c3ccccc3)c21
[C:1]-[C:2]1=[C:3](-[C;D1;H3:4])-[C;H0;D3;+0:5](=[O;H0;D1;+0:6])-[C:7]-[C:8]-1>>[C:1]-[C:2]1=[C:3](-[C;D1;H3:4])-[CH;D3;+0:5](-[OH;D1;+0:6])-[C:7]-[C:8]-1
51.5
[{"value": 51.5, "product": "COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
A mixture of 3-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranylmethyl)-2-methylcyclopent-2-en-1-one (0.17 g) and cerium trichloride heptahydrate (0.172 g) in tetrahydrofuran/methanol (12 mL, 4/1) was treated with sodium borohydride (0.035 g). After 0.5 hours, the reaction was diluted with ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
C1=CCCC1
C1=CCCC1
c1ccccc1.C1=CCCC1.c1ccc2c(c1)COC2
null
O1CCCC1.CO.C(C)(=O)OCC
null
0.5
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(=O)CC1)C(=O)OC2>O1CCCC1.CO.C(C)(=O)OCC>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(O)CC1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-503f176e7c5e44bebb7bb239234d51f6
C=COC1CCC(Cc2c(OC)c(C)c3c(c2OS(=O)(=O)c2ccc(C)cc2)C(=O)OC3)=C1C.COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(O)CC1)C(=O)OC2>>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(CC=O)CC1)C(=O)OC2
Cl(=O)(=O)(=O)[O-].[Li+].COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)OC=C)C.COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)O)C>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=C(C(CC1)CC=O)C
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C([O:28][CH:27]=[CH2:26])CC1)C(=O)OC2.O[CH:25]1[C:23]([CH3:24])=[C:22]([CH2:21][c:20]2[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]3[c:7]([c:8]2[O:9][S:10](=[O:11])(=[O:12])[c:13]2[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]2)[C:31](=[O:32])[O:33][CH2:34]3)[CH2:30][CH2:29]1>>[CH3:...
C=COC1CCC(Cc2c(OC)c(C)c3c(c2OS(=O)(=O)c2ccc(C)cc2)C(=O)OC3)=C1C.COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(O)CC1)C(=O)OC2
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(CC=O)CC1)C(=O)OC2
null
null
C([O-])(O)=O.[Na+].CCOCC.C(=C)OCC
Acylation
OtherReaction
4ac1d4e9ef6c92f6ee3fdeb6d6ffad4520472e6d1762372c8ec75a279a39fec6
d1039eb65b361cb7e491cf8dfd57a8623cae265c9dbfd4f1fbece64eeda0e199
O=C1OCc2ccc(CC3=CCCC3)c(OS(=O)(=O)c3ccccc3)c21
C-O-c1:c(-C):c2:c(:c(-O-S(=O)(=O)-c3:c:c:c(-C):c:c:3):c:1-C-C1=C(-C)-C(-[O;H0;D2;+0:1]-[CH;D2;+0:2]=[CH2;D1;+0:3])-C-C-1)-C(=O)-O-C-2.O-[CH;D3;+0:4]1-[C:5]-[C:6]-[C:7](-[C:8])=[C:9]-1-[C;D1;H3:10]>>[C:8]-[C:7]1=[C:9](-[C;D1;H3:10])-[CH;D3;+0:4](-[CH2;D2;+0:3]-[CH;D2;+0:2]=[O;H0;D1;+0:1])-[C:5]-[C:6]-1
null
[]
null
null
30
HOUR
To a solution of 3-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranylmethyl)-2-methylcyclopent-2-en-1-ol (0.157 g) in ethyl vinyl ether (10 mL) was added mercuric acetate (0.052 g). After stirring for 30 hours at ambient temperature, the reaction was diluted with ether and passed quickly thr...
10.6084/m9.figshare.5104873.v1
null
Tosylate.Ester.Ether.Ether.Secondary alcohol.Vinyl
Aldehyde
c1ccccc1.C1=CCCC1.c1ccc2c(c1)COC2.C1=CCCC1
C1=CCCC1
c1ccccc1.C1=CCCC1.c1ccc2c(c1)COC2
TsOH.HO-
C([O-])(O)=O.[Na+].CCOCC.C(=C)OCC
null
30
C=COC1CCC(Cc2c(OC)c(C)c3c(c2OS(=O)(=O)c2ccc(C)cc2)C(=O)OC3)=C1C.COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(O)CC1)C(=O)OC2>C([O-])(O)=O.[Na+].CCOCC.C(=C)OCC>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=C(C)C(CC=O)CC1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-aa7994f29d584866a4cbf0cebfe7ff59
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC=O)CC1)C(=O)OC2>>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC(=O)O)CC1)C(=O)OC2
Cl.C1(O)=CC(O)=CC=C1.COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=CC(CC1)(C)CC=O.Cl(=O)[O-].[Na+]>>COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=CC(CC1)(C)CC(=O)O
[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11])(=[O:12])[c:13]3[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]3)[c:20]1[CH2:21][C:22]1=[CH:23][C:24]([CH3:25])([CH2:26][CH:27]=[O:28])[CH2:30][CH2:31]1)[C:32](=[O:33])[O:34][CH2:35]2>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][S:10](=[O:11...
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC=O)CC1)C(=O)OC2
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC(=O)O)CC1)C(=O)OC2
null
null
O1CCOCC1.C(C)(=O)OCC
Oxidation
Oxidation of aldehydes to carboxylic acids
53d556378d4cb30c33d50a2e1886f8fba4abcbb7065d1faceeb5e5968b58008d
2f35b69536247c389825da7241226b4e568110d1cfe736c83136d58ad1c9dae2
O=C1OCc2ccc(CC3=CCCC3)c(OS(=O)(=O)c3ccccc3)c21
[C:1]=[C:2]-[C:3]-[C:4]-[CH;D2;+0:5]=[O;D1;H0:6]>>[C:1]=[C:2]-[C:3]-[C:4]-[C;H0;D3;+0:5](=[O;D1;H0:6])-[O;D1;H1:7]
null
[]
null
null
2
MINUTE
The 3-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy-5-isobenzofuranylmethyl)-1-methylcyclopent-2-en-1-ylacetaldehyde was dissolved in dioxane (8 mL) and pH 5 buffer (3 mL) and treated with resorcinol (0.10 g). To this mixture was then added sodium chlorite (0.080 g). After 2 minutes, the reaction was dil...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Carboxylic acid
null
null
c1ccccc1.C1=CCCC1.c1ccc2c(c1)COC2
Other
O1CCOCC1.C(C)(=O)OCC
null
0.033333
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC=O)CC1)C(=O)OC2>O1CCOCC1.C(C)(=O)OCC>COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC(=O)O)CC1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d044b48c5b3d413691e992c6ba016b16
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC(=O)O)CC1)C(=O)OC2>>COc1c(C)c2c(c(O)c1CC1=C(C)C(CC(=O)O)CC1)C(=O)OC2
COC1=C(C(=C2C(OCC2=C1C)=O)OS(=O)(=O)C1=CC=C(C=C1)C)CC1=CC(CC1)(C)CC(=O)O.O.[OH-].[Li+].CO.Cl>>OC1=C2C(OCC2=C(C(=C1CC1=C(C(CC1)CC(=O)O)C)OC)C)=O
Cc1ccc(S(=O)(=O)[O:9][c:8]2[c:7]3[c:6]([c:4]([CH3:5])[c:3]([O:2][CH3:1])[c:10]2[CH2:11][C:12]2=[CH:13][C:15]([CH3:14])([CH2:16][C:17](=[O:18])[OH:19])[CH2:20][CH2:21]2)[CH2:25][O:24][C:22]3=[O:23])cc1>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11][C:12]1=[C:13]([CH3:14])[CH:15]([CH2:16][C:17]...
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC(=O)O)CC1)C(=O)OC2
COc1c(C)c2c(c(O)c1CC1=C(C)C(CC(=O)O)CC1)C(=O)OC2
null
null
O.C(C)(=O)OCC
Functional Group Interconversion
OtherReaction
3b7ec937074c4678fd2476ef5eb15cf0d8cef638bcba24b7cfc4bedc8fe57bc6
f42bc74ea3e4acde8f757a6addaeeffa0b8900d54d39319d008e787b16303792
O=C1OCc2ccc(CC3=CCCC3)cc21
C-c1:c:c:c(-S(=O)(=O)-[O;H0;D2;+0:1]-[c:2](:[c:3]-[C:4]-[C:5]2=[CH;D2;+0:6]-[C;H0;D4;+0:7](-[CH3;D1;+0:8])(-[C:9]-[C:10](=[O;D1;H0:11])-[O;D1;H1:12])-[C:13]-[C:14]-2):[c:15]-[C:16](=[O;D1;H0:17])-[#8:18]):c:c:1>>[#8:18]-[C:16](=[O;D1;H0:17])-[c:15]:[c:2](-[OH;D1;+0:1]):[c:3]-[C:4]-[C:5]1=[C;H0;D3;+0:6](-[CH3;D1;+0:8])-...
null
[]
null
null
4
HOUR
The 3-(1,3-dihydro-6-methoxy-7-methyl-3-oxo-4-p-toluenesulfonyloxy -5-isobenzofuranylmethyl)-1-methylcyclopent-2-en-1-ylacetic acid obtained in Example ZC-1G was dissolved in a mixture of methanol (8 mL) and water (2 mL) and treated with lithium hydroxide monohydrate (0.15 g). After 4 hours, the reaction was diluted wi...
10.6084/m9.figshare.5104873.v1
null
Tosylate
Aromatic alcohol
c1ccccc1.C1=CCCC1
C1=CCCC1
C1=CCCC1.c1ccc2c(c1)COC2
TsOH.HO-
O.C(C)(=O)OCC
null
4
COc1c(C)c2c(c(OS(=O)(=O)c3ccc(C)cc3)c1CC1=CC(C)(CC(=O)O)CC1)C(=O)OC2>O.C(C)(=O)OCC>COc1c(C)c2c(c(O)c1CC1=C(C)C(CC(=O)O)CC1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-07739d7edf5d440498c0eb8a27b6ce82
CCOC(=O)C1CC/C(=C\Cc2c(O)c3c(c(C)c2OC)COC3=O)C1>>COc1c(C)c2c(c(O)c1C/C=C1\CCC(C(=O)O)C1)C(=O)OC2
OC1=C2C(OCC2=C(C(=C1C\C=C/1\CC(CC1)C(=O)OCC)OC)C)=O>>OC1=C2C(OCC2=C(C(=C1C\C=C/1\CC(CC1)C(=O)O)OC)C)=O
CC[O:19][C:17]([CH:16]1[CH2:15][CH2:14]/[C:13](=[CH:12]\[CH2:11][c:10]2[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]3[c:7]([c:8]2[OH:9])[C:21](=[O:22])[O:23][CH2:24]3)[CH2:20]1)=[O:18]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11]/[CH:12]=[C:13]1\[CH2:14][CH2:15][CH:16]([C:17](=[O:18])[OH:19])[CH2:...
CCOC(=O)C1CC/C(=C\Cc2c(O)c3c(c(C)c2OC)COC3=O)C1
COc1c(C)c2c(c(O)c1C/C=C1\CCC(C(=O)O)C1)C(=O)OC2
null
null
CCCCCC.ClCCl
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccc(CC=C3CCCC3)cc21
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
By following the procedure of Example ZA-6A and substituting methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2,4-dimethyl-4-hexenoate with ethyl (E)-3-[2-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)ethylidene]cyclopentane -1-carboxylate (prepared e.g, as described w...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CCCC1.c1ccc2c(c1)COC2
Other
CCCCCC.ClCCl
null
null
CCOC(=O)C1CC/C(=C\Cc2c(O)c3c(c(C)c2OC)COC3=O)C1>CCCCCC.ClCCl>COc1c(C)c2c(c(O)c1C/C=C1\CCC(C(=O)O)C1)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-7820518b8590443d8b86b8ccf4ea84e0
C=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.CC(=O)OC(C)=O>>C=CCc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
C(C)(=O)OC(C)=O.C(C=C)C=1C(=C2C(OCC2=C(C1OC)C)=O)O[Si](C)(C)C(C)(C)C>>C(C)(=O)OC1=C2C(OCC2=C(C(=C1CC=C)OC)C)=O
CC(C)(C)[Si](C)(C)[O:13][c:12]1[c:4]([CH2:3][CH:2]=[CH2:1])[c:5]([O:6][CH3:7])[c:8]([CH3:9])[c:10]2[c:11]1[C:17](=[O:18])[O:19][CH2:20]2.CC(=O)O[C:14]([CH3:15])=[O:16]>>[CH2:1]=[CH:2][CH2:3][c:4]1[c:5]([O:6][CH3:7])[c:8]([CH3:9])[c:10]2[c:11]([c:12]1[O:13][C:14]([CH3:15])=[O:16])[C:17](=[O:18])[O:19][CH2:20]2
C=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.CC(=O)OC(C)=O
C=CCc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
null
null
C(C)(=O)O
Acylation
OtherReaction
dc2e4916eb1e0336df7600ab21ace635942c529e40899dfc51f11e1099dafec6
cd167da0128b84942308a2361251a58b9a15c9502e99a9a75e3e1ddf830ff991
O=C1OCc2ccccc21
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](=[O;D1;H0:6])-[#8:7].C-C(=O)-O-[C;H0;D3;+0:8](-[C;D1;H3:9])=[O;D1;H0:10]>>[#8:7]-[C:5](=[O;D1;H0:6])-[c:4]:[c:2](-[O;H0;D2;+0:1]-[C;H0;D3;+0:8](-[C;D1;H3:9])=[O;D1;H0:10]):[c:3]
null
[]
null
null
null
null
A solution of 5-allyl-4-tert-butyldimethylsilyloxy-1,3-dihydro -6-methoxy-7-methyl-3-oxoisobenzofuran [(J. W. Patterson and G. Huang, Chemical Communications, 1579 (1991)] (7.5 g) in acetic acid (95 ml) and acetic anhydride (95 ml) was refluxed for 18 hours, then cooled and poured into ice water. The solution was extra...
10.6084/m9.figshare.5104873.v1
null
Anhydride.TMS ether protective group
Ester
null
null
c1ccc2c(c1)COC2
HO-
C(C)(=O)O
null
null
C=CCc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2.CC(=O)OC(C)=O>C(C)(=O)O>C=CCc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-9b1df400bb1d44a4868aff1a360a7ffa
C=CCc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2.COC(=O)c1cccc(C)c1Br>>COC(=O)c1cccc(C)c1/C=C/Cc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
C(C)(=O)OC1=C2C(OCC2=C(C(=C1CC=C)OC)C)=O.BrC1=C(C(=O)OC)C=CC=C1C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.Cl>>C(C)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C/C1=C(C(=O)OC)C=CC=C1C)OC)C)=O
[CH2:12]=[CH:13][CH2:14][c:15]1[c:16]([O:17][CH3:18])[c:19]([CH3:20])[c:21]2[c:22]([c:23]1[O:24][C:25]([CH3:26])=[O:27])[C:28](=[O:29])[O:30][CH2:31]2.Br[c:11]1[c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:6][cH:7][cH:8][c:9]1[CH3:10]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][cH:8][c:9]([CH3:10])[c:11]1/[CH:12]=[CH:13]/[CH2:1...
C=CCc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2.COC(=O)c1cccc(C)c1Br
COC(=O)c1cccc(C)c1/C=C/Cc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
null
C([O-])([O-])=O.[Ag+2].C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-]
CN(C=O)C
C-C Coupling
OtherReaction
2d4a44695e29e4a9ab430c3b66736ad86dd99247e7216f16f3ca137abca78747
df8442c9f2045421fb18548edb9c6acaeb9710f63e741d9f72e0000ca35c948a
O=C1OCc2ccc(C/C=C/c3ccccc3)cc21
Br-[c;H0;D3;+0:1](:[c:2](-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6]):[c:7]):[c:8](-[C;D1;H3:9]):[c:10].[C:11]-[C:12]=[CH2;D1;+0:13]>>[C:11]/[C:12]=[CH;D2;+0:13]/[c;H0;D3;+0:1](:[c:2](-[C:3](=[O;D1;H0:4])-[#8:5]-[C;D1;H3:6]):[c:7]):[c:8](-[C;D1;H3:9]):[c:10]
null
[]
100
CELSIUS
6
HOUR
4-Acetoxy-5-allyl-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran (0.6 g), methyl 2-bromo-3-methylbenzoate (0.92 g), silver carbonate (1.3 g), palladium acetate (0.1 g), triphenylphosphine (0.14 g) and dimethylformamide (70 ml) were heated with stirring at 100° C. for 6 hours, then stirred at ambient temperature for ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Allyl
null
c1ccccc1
c1ccccc1
c1ccccc1.c1ccc2c(c1)COC2
HBr
C([O-])([O-])=O.[Ag+2].C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].CN(C=O)C
100
6
C=CCc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2.COC(=O)c1cccc(C)c1Br>C([O-])([O-])=O.[Ag+2].C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].CN(C=O)C>COC(=O)c1cccc(C)c1/C=C/Cc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-47c6f01829024b97bbd90d3a8cd2c7d7
COC(=O)c1cccc(C)c1/C=C/Cc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2>>COc1c(C)c2c(c(OC(C)=O)c1C/C=C/c1c(C)cccc1C(=O)O)C(=O)OC2
C(C)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C/C1=C(C(=O)OC)C=CC=C1C)OC)C)=O.[OH-].[Li+].Cl>>C(C)(=O)OC1=C2C(OCC2=C(C(=C1C/C=C/C1=C(C(=O)O)C=CC=C1C)OC)C)=O
C[O:26][C:24]([c:23]1[c:17](/[CH:16]=[CH:15]/[CH2:14][c:13]2[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]3[c:7]([c:8]2[O:9][C:10]([CH3:11])=[O:12])[C:27](=[O:28])[O:29][CH2:30]3)[c:18]([CH3:19])[cH:20][cH:21][cH:22]1)=[O:25]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([O:9][C:10]([CH3:11])=[O:12])[c:13]1[CH2:14]/[CH:15...
COC(=O)c1cccc(C)c1/C=C/Cc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2
COc1c(C)c2c(c(OC(C)=O)c1C/C=C/c1c(C)cccc1C(=O)O)C(=O)OC2
null
null
O.CO
Deprotection
Ester saponification (methyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccc(C/C=C/c3ccccc3)cc21
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]
null
[]
null
null
null
null
A solution of methyl (E)-2-[3-(4-acetoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-prop-1-en-1-yl]-3-methylbenzoate (0.1 g) and lithium hydroxide (0.06 g) in methanol (1 ml) and water (1 ml) was heated at 70° C. for 48 hours. The solution was cooled and poured into water, then acidified with 2N hydrochlor...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccc2c(c1)COC2
Other
O.CO
null
null
COC(=O)c1cccc(C)c1/C=C/Cc1c(OC)c(C)c2c(c1OC(C)=O)C(=O)OC2>O.CO>COc1c(C)c2c(c(OC(C)=O)c1C/C=C/c1c(C)cccc1C(=O)O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-b4a749ba1a50456f8151b855f22ae779
CC(C)(C)C(=O)O.COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)/C(C)=C/CC(C)C(C)(O[SiH3])C(C)(C)C)C(=O)OC2>>CCOC(=O)CC(CCCO[Si](C)(C)C(C)(C)C)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1CC(/C(=C/CC(C(C(C)(C)C)(O[SiH3])C)C)/C)O)OC)C)=O.C(C(C)(C)C)(=O)O>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCO[Si](C)(C)C(C)(C)C)\C)OC)C)=O
[CH3:1][C:2]([C:4]([OH:3])=[O:5])([CH3:13])[CH3:14].C[CH:9]([C:7](O[SiH3:12])([CH3:6])[C:15]([CH3:16])([CH3:17])[CH3:18])[CH2:8]/[CH:21]=[C:19](/[CH:10]([OH:11])[CH2:22][c:23]1[c:24]([O:25][CH3:26])[c:27]([CH3:28])[c:29]2[c:30]([c:31]1[O:32][Si:33]([CH3:34])([CH3:35])[C:36]([CH3:37])([CH3:38])[CH3:39])[C:40](=[O:41])[O...
CC(C)(C)C(=O)O.COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)/C(C)=C/CC(C)C(C)(O[SiH3])C(C)(C)C)C(=O)OC2
CCOC(=O)CC(CCCO[Si](C)(C)C(C)(C)C)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
null
CCOCC.C(C)(OCC)(OCC)OCC
C-C Coupling
OtherReaction
a1a7af0c08b7f601e7365d00f615cb09e77e1fb8a8adb2a8aed8c2fb085907d6
d768a9cd2aa0fcd146aba6171d08b2a3f65cd24f010103bca90ec50d75a81782
O=C1OCc2ccccc21
C-[CH;D3;+0:1](-[CH2;D2;+0:2]/[CH;D2;+0:3]=[C;H0;D3;+0:4](\[C;D1;H3:5])-[CH;D3;+0:6](-[OH;D1;+0:7])-[CH2;D2;+0:8]-[c:9](:[c:10]):[c:11])-[C;H0;D4;+0:12](-[CH3;D1;+0:13])(-O-[SiH3;D1;+0:14])-[C;H0;D4;+0:15](-[C;D1;H3:16])(-[C;D1;H3:17])-[C;D1;H3:18].[C;D1;H3:19]-[C;H0;D4;+0:20](-[CH3;D1;+0:21])(-[CH3;D1;+0:22])-[C;H0;D3...
276.5
[{"value": 276.5, "product": "[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCO[Si](C)(C)C(C)(C)C)\\C)OC)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
(E)-7-(4-tert-butyldimethylsilyloxy-1,3-dihydro-6-methoxy-7-methyl -3-oxoisobenzofuran-5-yl)-1-tert-butyldimethyl-silyloxy-6-hydroxy -5-methylhept-4-ene (4.74 g) was dissolved in triethyl orthoacetate (76 ml) and pivalic acid (171 mg) was added. The solution was placed in an oil bath preheated to 130° C., and stirred f...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol
Ester.TMS ether protective group
null
null
c1ccc2c(c1)COC2
HO-
CCOCC.C(C)(OCC)(OCC)OCC
null
0.5
CC(C)(C)C(=O)O.COc1c(C)c2c(c(O[Si](C)(C)C(C)(C)C)c1CC(O)/C(C)=C/CC(C)C(C)(O[SiH3])C(C)(C)C)C(=O)OC2>CCOCC.C(C)(OCC)(OCC)OCC>CCOC(=O)CC(CCCO[Si](C)(C)C(C)(C)C)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-836ced56c8c24fdfb72bfddef7a5f7f9
CCOC(=O)CC(CCCO[Si](C)(C)C(C)(C)C)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>CCOC(=O)CC(CCCO)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCO[Si](C)(C)C(C)(C)C)\C)OC)C)=O>>[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCO)\C)OC)C)=O
CC(C)(C)[Si](C)(C)[O:11][CH2:10][CH2:9][CH2:8][CH:7]([CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5])/[C:12]([CH3:13])=[CH:14]/[CH2:15][c:16]1[c:17]([O:18][CH3:19])[c:20]([CH3:21])[c:22]2[c:23]([c:24]1[O:25][Si:26]([CH3:27])([CH3:28])[C:29]([CH3:30])([CH3:31])[CH3:32])[C:33](=[O:34])[O:35][CH2:36]2>>[CH3:1][CH2:2][O:3][C:4](=[...
CCOC(=O)CC(CCCO[Si](C)(C)C(C)(C)C)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
CCOC(=O)CC(CCCO)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
null
null
C(C)#N
Deprotection
Alcohol deprotection from silyl ethers
6ff8c9c41093ab5237b871dd4689ba6431022d615e227d3774901a983c846e4b
84d9f5b4e7757c58e584c26c7d52c9a3f594fbcb0c0d22f34765a93a932fcd5b
O=C1OCc2ccccc21
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[OH;D1;+0:1]
87.7
[{"value": 87.7, "product": "[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCO)\\C)OC)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
Ethyl (E) 6-(4-tert-butyldimethylsilyloxy-1,3-dihydro-6-methoxy -7-methyl-3-oxo-isobenzofuran-5-yl)-3-(3-tert-butyldimethylsilyloxypropyl) -4-methylhex-4-enoate (2.92 g) was dissolved in acetonitrile (50 ml). To this was added a solution of 40% aqueous HF (5 ml) in acetonitrile (45 ml), and the reaction mixture stirred...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Primary alcohol
null
null
c1ccc2c(c1)COC2
Other
C(C)#N
null
0.166667
CCOC(=O)CC(CCCO[Si](C)(C)C(C)(C)C)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>C(C)#N>CCOC(=O)CC(CCCO)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0320830997a041e49aaec6fb21a36af9
CCOC(=O)CC(CCCBr)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>>CCOC(=O)CC(CCCBr)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
[Si](C)(C)(C(C)(C)C)OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCBr)\C)OC)C)=O.O.O.O.[F-].C(CCC)[N+](CCCC)(CCCC)CCCC>>OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCBr)\C)OC)C)=O
CC(C)(C)[Si](C)(C)[O:18][c:17]1[c:16]([CH2:15]/[CH:14]=[C:12](/[CH:7]([CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:8][CH2:9][CH2:10][Br:11])[CH3:13])[c:23]([O:24][CH3:25])[c:21]([CH3:22])[c:20]2[c:19]1[C:28](=[O:29])[O:27][CH2:26]2>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH:7]([CH2:8][CH2:9][CH2:10][Br:11])/[C:12]([CH...
CCOC(=O)CC(CCCBr)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2
CCOC(=O)CC(CCCBr)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
null
null
CCOCC.C1CCOC1
Deprotection
Alcohol deprotection from silyl ethers
e70131badc7d7d580ed75b2dfb3ce6df2a5f496b2119611cf5354e1267babe73
b09ece7bccc3ff762f4ff5407ad846fffba6d6a63735853c86a86d29904f54ed
O=C1OCc2ccccc21
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]-[C:5](=[O;D1;H0:6])-[#8:7]>>[#8:7]-[C:5](=[O;D1;H0:6])-[c:4]:[c:2](-[OH;D1;+0:1]):[c:3]
62.2
[{"value": 62.2, "product": "OC1=C2C(OCC2=C(C(=C1C/C=C(/C(CC(=O)OCC)CCCBr)\\C)OC)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
15
MINUTE
A solution of of ethyl (E) 6-(4-tert-butyldimethylsilyloxy -1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl) -3-(3-bromopropyl)-4-methylhex-4-enoate (1.62 g) was dissolved in THF (25 ml), cooled to 0° C., and a solution of tetrabutylammonium fluoride trihydrate (919 mg) in THF (5 ml) was added. The reaction was ...
10.6084/m9.figshare.5104873.v1
null
TMS ether protective group
Aromatic alcohol
null
null
c1ccc2c(c1)COC2
Other
CCOCC.C1CCOC1
0
0.25
CCOC(=O)CC(CCCBr)/C(C)=C/Cc1c(OC)c(C)c2c(c1O[Si](C)(C)C(C)(C)C)C(=O)OC2>CCOCC.C1CCOC1>CCOC(=O)CC(CCCBr)/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-8a7d68a9fc10428b81c893f585c53f4a
CCOC(=O)C1CCCC1/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>>COc1c(C)c2c(c(O)c1C/C=C(\C)C1CCCC1C(=O)O)C(=O)OC2
OC1=C2C(OCC2=C(C(=C1C/C=C(\C)/C1C(CCC1)C(=O)OCC)OC)C)=O>>OC1=C2C(OCC2=C(C(=C1C/C=C(\C)/C1C(CCC1)C(=O)O)OC)C)=O
CC[O:22][C:20]([CH:19]1[CH:15](/[C:13](=[CH:12]/[CH2:11][c:10]2[c:3]([O:2][CH3:1])[c:4]([CH3:5])[c:6]3[c:7]([c:8]2[OH:9])[C:23](=[O:24])[O:25][CH2:26]3)[CH3:14])[CH2:16][CH2:17][CH2:18]1)=[O:21]>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]2[c:7]([c:8]([OH:9])[c:10]1[CH2:11]/[CH:12]=[C:13](\[CH3:14])[CH:15]1[CH2:16][CH2:17][C...
CCOC(=O)C1CCCC1/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O
COc1c(C)c2c(c(O)c1C/C=C(\C)C1CCCC1C(=O)O)C(=O)OC2
null
null
CCCCCC.C(C)(=O)OCC
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=C1OCc2ccc(CC=CC3CCCC3)cc21
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
By following the procedure of Example ZA-6A and substituting methyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxoisobenzofuran -5-yl)-2,4-dimethyl-4-hexenoate with ethyl (E)-2-[-3-(4-hydroxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-1-methylpropenyl ]-cyclopentane-carboxylate and compounds of Form...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CCCC1.c1ccc2c(c1)COC2
Other
CCCCCC.C(C)(=O)OCC
null
null
CCOC(=O)C1CCCC1/C(C)=C/Cc1c(O)c2c(c(C)c1OC)COC2=O>CCCCCC.C(C)(=O)OCC>COc1c(C)c2c(c(O)c1C/C=C(\C)C1CCCC1C(=O)O)C(=O)OC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ab73c212c79c45b8805584012da837d6
CC1=C[C@H]2O[C@@H]3C[C@H]4OC(=O)/C=C\C=C\C(=O)OCC[C@@H](C)[C@H](O)C(=O)OC[C@@]2(CC1)[C@]4(C)[C@]31CO1>>CC1=C[C@H]2O[C@@H]3CC[C@@](C)(C3C)[C@@]2(C)CC1
[Se](=O)=O.C[C@@H]1CCOC(=O)/C=C/C=C\C(=O)O[C@@H]2C[C@@H]3[C@]4([C@]2([C@]5(CCC(=C[C@H]5O3)C)COC(=O)[C@H]1O)C)CO4>>CC1[C@H]2CC[C@@]1([C@]3(CCC(=C[C@H]3O2)C)C)C
C[C@@H]1CCOC(=O)/C=C/C=C\C(=O)O[C@@H:8]2[CH2:7][C@H:6]3[O:5][C@@H:4]4[CH:3]=[C:2]([CH3:1])[CH2:16][CH2:15][C@@:13]4([C@:9]2([CH3:10])[C@@:11]32O[CH2:12]2)[CH2:14]OC(=O)[C@H]1O>>[CH3:1][C:2]1=[CH:3][C@H:4]2[O:5][C@@H:6]3[CH2:7][CH2:8][C@@:9]([CH3:10])([CH:11]3[CH3:12])[C@@:13]2([CH3:14])[CH2:15][CH2:16]1
CC1=C[C@H]2O[C@@H]3C[C@H]4OC(=O)/C=C\C=C\C(=O)OCC[C@@H](C)[C@H](O)C(=O)OC[C@@]2(CC1)[C@]4(C)[C@]31CO1
CC1=C[C@H]2O[C@@H]3CC[C@@](C)(C3C)[C@@]2(C)CC1
null
null
null
Reduction
OtherReaction
eab71b612ede83a39b8bdbe09aced4e88043cd674701b49a41ec319f03026e88
0d48a27d606bb0a7b9f1bb881aa368ce08db06636d6bc6626511bfbcfa12a5d7
C1=C[C@H]2O[C@@H]3CCC(C3)C2CC1
null
null
[]
null
null
null
null
The trichothecene therapeutic agent 16-oxo verrucarin A is prepared by selenium dioxide oxidation of verrucarin A. The MAb hydrazide is then reacted with 16-oxo verrucarin A at 4° C. overnight with agitation, thereby yielding a unique Schiff base-linked targeting protein having the following structure: ##STR19## Condit...
10.6084/m9.figshare.5104873.v1
null
Ester.Ester.Ester.Ether.Secondary alcohol.Conjugated diene
null
C1=C[C@H]2O[C@@H]3C[C@H]4OC/C=C\C=C\COCCCCCOC[C@@]2(CC1)[C@@H]4[C@]31CO1
C1=C[C@H]2O[C@@H]3CC[C@@H](C3)[C@H]2CC1
C1=C[C@H]2O[C@@H]3CC[C@@H](C3)[C@H]2CC1
HO-
null
null
null
CC1=C[C@H]2O[C@@H]3C[C@H]4OC(=O)/C=C\C=C\C(=O)OCC[C@@H](C)[C@H](O)C(=O)OC[C@@]2(CC1)[C@]4(C)[C@]31CO1>>CC1=C[C@H]2O[C@@H]3CC[C@@](C)(C3C)[C@@]2(C)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f301d0b9494940d59d0901c5a8aebf22
C#CCCC.O=c1[nH]c(=O)n([C@H]2C[C@H](O)[C@@H](CO)O2)cc1I>>CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
CO.IC=1C(NC(N([C@H]2C[C@H](O)[C@@H](CO)O2)C1)=O)=O.C#CCCC.C([O-])(O)=O>>C(#CCCC)C=1C(NC(N([C@H]2C[C@H](O)[C@@H](CO)O2)C1)=O)=O
[CH3:1][CH2:2][CH2:3][C:4]#[CH:5].I[c:6]1[cH:7][n:8]([C@H:9]2[CH2:10][C@H:11]([OH:12])[C@@H:13]([CH2:14][OH:15])[O:16]2)[c:17](=[O:18])[nH:19][c:20]1=[O:21]>>[CH3:1][CH2:2][CH2:3][C:4]#[C:5][c:6]1[cH:7][n:8]([C@H:9]2[CH2:10][C@H:11]([OH:12])[C@@H:13]([CH2:14][OH:15])[O:16]2)[c:17](=[O:18])[nH:19][c:20]1=[O:21]
C#CCCC.O=c1[nH]c(=O)n([C@H]2C[C@H](O)[C@@H](CO)O2)cc1I
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
null
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Cu]I
C(Cl)Cl
C-C Coupling
Sonogashira alkyne_aryl halide
6c841971a35ffd50215936cda19c192218792b140679c95a1b7a8fa56d8a741b
305eca0fd2975da49e7f69e4edfb9dc1cbce82513954bc5a73be3289e70e5f76
O=c1ccn([C@H]2CCCO2)c(=O)[nH]1
I-[c;H0;D3;+0:1]1:[c:2]:[#7;a:3](-[C:4]-[#8:5]):[c:6]:[#7;a:7]:[c:8]:1=[O;D1;H0:9].[C:10]-[C:11]#[CH;D1;+0:12]>>[#8:5]-[C:4]-[#7;a:3]1:[c:6]:[#7;a:7]:[c:8](=[O;D1;H0:9]):[c;H0;D3;+0:1](-[C;H0;D2;+0:12]#[C:11]-[C:10]):[c:2]:1
81.9
[{"value": 81.9, "product": "C(#CCCC)C=1C(NC(N([C@H]2C[C@H](O)[C@@H](CO)O2)C1)=O)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
26
HOUR
This compound was prepared by the same procedure that Hobbs, F. W. J., J Org Chem (1989) 54: 3420-3422, used for the preparation of other alkynyl substituted nucleosides. A mixture of 30.0 g (84.7 mmol) of 5-iodo-2'deoxyuridine (purchased from Sigma), 23.6 mL of 1-pentyne (Aldrich), 9.79 g of tetrakis (triphenylphosphi...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Alkyne
Alkyne
c1cncnc1
c1cncnc1
c1cncnc1.C1CCOC1
HI
[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Cu]I.C(Cl)Cl
null
26
C#CCCC.O=c1[nH]c(=O)n([C@H]2C[C@H](O)[C@@H](CO)O2)cc1I>[Pd].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Cu]I.C(Cl)Cl>CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-4fc6b35319144df28c3a7ce2cc497b35
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O.COc1ccc(C(Cl)(c2ccccc2)c2ccc(OC)cc2)cc1>>CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](COC(c3ccccc3)(c3ccc(OC)cc3)c3ccc(OC)cc3)O2)c(=O)[nH]c1=O
C(#CCCC)C=1C(NC(N([C@H]2C[C@H](O)[C@@H](CO)O2)C1)=O)=O.COC1=CC=C(C(C2=CC=C(C=C2)OC)(C2=CC=CC=C2)Cl)C=C1>>COC1=CC=C(C(C2=CC=C(C=C2)OC)(C2=CC=CC=C2)OC[C@@H]2[C@H](C[C@@H](O2)N2C(=O)NC(=O)C(=C2)C#CCCC)O)C=C1
[CH3:1][CH2:2][CH2:3][C:4]#[C:5][c:6]1[cH:7][n:8]([C@H:9]2[CH2:10][C@H:11]([OH:12])[C@@H:13]([CH2:14][OH:15])[O:39]2)[c:40](=[O:41])[nH:42][c:43]1=[O:44].Cl[C:16]([c:17]1[cH:18][cH:19][cH:20][cH:21][cH:22]1)([c:23]1[cH:24][cH:25][c:26]([O:27][CH3:28])[cH:29][cH:30]1)[c:31]1[cH:32][cH:33][c:34]([O:35][CH3:36])[cH:37][cH...
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O.COc1ccc(C(Cl)(c2ccccc2)c2ccc(OC)cc2)cc1
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](COC(c3ccccc3)(c3ccc(OC)cc3)c3ccc(OC)cc3)O2)c(=O)[nH]c1=O
null
null
N1=CC=CC=C1
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
fb955127af596450632db904a0236d35e158107f202af7adbe96e225ff5ada1f
5adfb0e9c2ca3c5afac2c4b206fb6fda83b92f44074f2a75e26f913c192bc169
O=c1ccn([C@H]2CC[C@@H](COC(c3ccccc3)(c3ccccc3)c3ccccc3)O2)c(=O)[nH]1
Cl-[C;H0;D4;+0:1](-[c:2](:[c:3]):[c:4])(-[c:5](:[c:6]):[c:7])-[c:8](:[c:9]):[c:10].[#8:11]-[C:12]-[C:13]-[OH;D1;+0:14]>>[#8:11]-[C:12]-[C:13]-[O;H0;D2;+0:14]-[C;H0;D4;+0:1](-[c:2](:[c:3]):[c:4])(-[c:5](:[c:6]):[c:7])-[c:8](:[c:9]):[c:10]
54.5
[{"value": 52.9, "product": "COC1=CC=C(C(C2=CC=C(C=C2)OC)(C2=CC=CC=C2)OC[C@@H]2[C@H](C[C@@H](O2)N2C(=O)NC(=O)C(=C2)C#CCCC)O)C=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 54.5, "product": "COC1=CC=C(C(C2=CC=C(C=C2)OC)(C2=CC=CC=C2)OC[C@@H]2[C@H](C[C@@H](O2)N2C(=O)NC(=O)C(=C2)C#CCCC)O)C=C1", "details":...
null
null
17
HOUR
To 20.4 g (69.3 mmol) of 5-(1-pentynyl)-2'-deoxyuridine in 300 mL of dry pyridine was added 22.8 g of 4,4'-dimethoxytrityl chloride. The reaction was stirred for 17 h at room temperature and then concentrated. The residue was taken up in CH2Cl2 and washed twice with 0.5% aqueous NaHCO3, dried (Na2SO4), filtered, and co...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Primary alcohol
Ether
null
null
c1cncnc1.C1CCOC1.c1ccccc1.c1ccccc1.c1ccccc1
HCl
N1=CC=CC=C1
null
17
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O.COc1ccc(C(Cl)(c2ccccc2)c2ccc(OC)cc2)cc1>N1=CC=CC=C1>CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](COC(c3ccccc3)(c3ccc(OC)cc3)c3ccc(OC)cc3)O2)c(=O)[nH]c1=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-775c308cf3824ac2aaae6e5316af307d
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O>>CCCCCc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
C(#CCCC)C=1C(NC(N([C@H]2C[C@H](O)[C@@H](CO)O2)C1)=O)=O>>C(CCCC)C=1C(NC(N([C@H]2C[C@H](O)[C@@H](CO)O2)C1)=O)=O
[CH3:1][CH2:2][CH2:3][C:4]#[C:5][c:6]1[cH:7][n:8]([C@H:9]2[CH2:10][C@H:11]([OH:12])[C@@H:13]([CH2:14][OH:15])[O:16]2)[c:17](=[O:18])[nH:19][c:20]1=[O:21]>>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][c:6]1[cH:7][n:8]([C@H:9]2[CH2:10][C@H:11]([OH:12])[C@@H:13]([CH2:14][OH:15])[O:16]2)[c:17](=[O:18])[nH:19][c:20]1=[O:21]
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
CCCCCc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
null
[Pd]
CO
Reduction
OtherReaction
2bb8d5b532a2781e0a7c069a5cd3e8a7e8d44660c0ec1d9e17c04d8ba2cb383b
1990560e9c55934bde8ca0feaed9c61d80f37f94f0cf240a9929dc374d0a33aa
O=c1ccn([C@H]2CCCO2)c(=O)[nH]1
[#8:1]-[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6](=[O;D1;H0:7]):[c:8](-[C;H0;D2;+0:9]#[C;H0;D2;+0:10]-[C:11]-[C:12]):[c:13]:1>>[#8:1]-[C:2]-[#7;a:3]1:[c:4]:[#7;a:5]:[c:6](=[O;D1;H0:7]):[c:8](-[CH2;D2;+0:9]-[CH2;D2;+0:10]-[C:11]-[C:12]):[c:13]:1
null
[]
null
null
14
HOUR
To a solution of 1.03 g (3.50 mmol) of 5-(1-pentynyl)-2'-deoxyuridine in 25 mL of MeOH was added a catalytic amount of 10% Pd on charcoal. The mixture was hydrogenated under 300 psi of H2 for 14 h at room temperature. The mixture was filtered through Celite and concentrated, affording a quantitative yield of product. C...
10.6084/m9.figshare.5104873.v1
null
Alkyne
null
null
null
c1cncnc1.C1CCOC1
null
[Pd].CO
null
14
CCCC#Cc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O>[Pd].CO>CCCCCc1cn([C@H]2C[C@H](O)[C@@H](CO)O2)c(=O)[nH]c1=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1599ec65fdd54d67a7b447137a9c1a30
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@]1(O)C(C)=O>>CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@H]1O
Br[C@H]1[C@@H](O[C@@H]([C@]1(O)C(C)=O)COC(C)=O)N1C(=O)NC(=O)C(=C1)C.O.NN.Cl>>Br[C@H]1[C@@H](O[C@@H]([C@H]1O)COC(C)=O)N1C(=O)NC(=O)C(=C1)C
CC(=O)[C@@:20]1([OH:21])[C@@H:6]([CH2:5][O:4][C:2]([CH3:1])=[O:3])[O:7][C@@H:8]([n:9]2[cH:10][c:11]([CH3:12])[c:13](=[O:14])[nH:15][c:16]2=[O:17])[C@@H:18]1[Br:19]>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][C@H:6]1[O:7][C@@H:8]([n:9]2[cH:10][c:11]([CH3:12])[c:13](=[O:14])[nH:15][c:16]2=[O:17])[C@H:18]([Br:19])[C@@H:20]1[OH:21]
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@]1(O)C(C)=O
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@H]1O
null
null
O.C(C)#N
Reduction
OtherReaction
43d88ce45446e857bff66cf064de0c45cea59f153344a8de8b37df2ca8b00fba
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
O=c1ccn([C@H]2CCCO2)c(=O)[nH]1
C-C(=O)-[C@;H0;D4;+0:1]1(-[O;D1;H1:2])-[C:3](-[Br;D1;H0:4])-[C:5]-[#8:6]-[C:7]-1-[C:8]>>[Br;D1;H0:4]-[C:3]1-[C:5]-[#8:6]-[C:7](-[C:8])-[C@H;D3;+0:1]-1-[O;D1;H1:2]
92.9
[{"value": 76.0, "product": "Br[C@H]1[C@@H](O[C@@H]([C@H]1O)COC(C)=O)N1C(=O)NC(=O)C(=C1)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 92.9, "product": "Br[C@H]1[C@@H](O[C@@H]([C@H]1O)COC(C)=O)N1C(=O)NC(=O)C(=C1)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
null
null
400 ml of acetonitrile and 2.16 g (3 equivalents) of water were added to 16.2 g (40.0 mmol) of 2'-deoxy-2'-bromo-3',5'-O-diacetyl-5-methyluridine, and the mixture was stirred. The resulting solution was cooled to 0° C., 6.01 g (3 equivalents) of hydrazine monohydrate were added thereto, and the mixture was reacted for ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
C1CCOC1
C1CCOC1
C1CCOC1.c1cncnc1
HO-
O.C(C)#N
0
null
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@]1(O)C(C)=O>O.C(C)#N>CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@H]1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3257e360c2f74fb392e93d05e85ea09c
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@H]1O>>CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1O
Br[C@H]1[C@@H](O[C@@H]([C@H]1O)COC(C)=O)N1C(=O)NC(=O)C(=C1)C.C(C)(=O)[O-].[Na+].[H][H]>>C(C)(=O)OC[C@@H]1[C@H](C[C@@H](O1)N1C(=O)NC(=O)C(C)=C1)O
Br[C@H:18]1[C@H:8]([n:9]2[cH:10][c:11]([CH3:12])[c:13](=[O:14])[nH:15][c:16]2=[O:17])[O:7][C@H:6]([CH2:5][O:4][C:2]([CH3:1])=[O:3])[C@H:19]1[OH:20]>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][C@H:6]1[O:7][C@@H:8]([n:9]2[cH:10][c:11]([CH3:12])[c:13](=[O:14])[nH:15][c:16]2=[O:17])[CH2:18][C@@H:19]1[OH:20]
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@H]1O
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1O
null
S(=O)(=O)([O-])[O-].[Ba+2].[Pd+2].S(=O)(=O)([O-])[O-]
CO
Functional Group Interconversion
Dehalogenation
2c0570e07732844d84f39e96c7630be6331c1effa6291ee67002cb43b6c323f3
6e8d13230370538f865fe4c85906dd6cad07c6cb5b152c1d96823b885b960ee6
O=c1ccn([C@H]2CCCO2)c(=O)[nH]1
Br-[C@@H;D3;+0:1]1-[C:2](-[O;D1;H1:3])-[C:4]-[#8:5]-[C:6]-1-[#7;a:7]>>[#7;a:7]-[C:6]1-[#8:5]-[C:4]-[C:2](-[O;D1;H1:3])-[CH2;D2;+0:1]-1
38.1
[{"value": 38.1, "product": "C(C)(=O)OC[C@@H]1[C@H](C[C@@H](O1)N1C(=O)NC(=O)C(C)=C1)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 38.1, "product": "C(C)(=O)OC[C@@H]1[C@H](C[C@@H](O1)N1C(=O)NC(=O)C(C)=C1)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
12.47 g (28.1 mmol) of 2'-deoxy-2'-bromo-5'-O-acetyl-5-methyluridine were dissolved in 240 ml of methanol, and 6.91 g (3 equivalents) of sodium acetate were added thereto. To the reaction mixture, were added 1.25 g of 5% palladium-barium sulfate catalyst (0.1 equivalent). Then, the reaction system was filled with hydro...
10.6084/m9.figshare.5104873.v1
null
Secondary halide
null
C1CCOC1
C1CCOC1
C1CCOC1.c1cncnc1
Br-
S(=O)(=O)([O-])[O-].[Ba+2].[Pd+2].S(=O)(=O)([O-])[O-].CO
null
null
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)[C@H](Br)[C@@H]1O>S(=O)(=O)([O-])[O-].[Ba+2].[Pd+2].S(=O)(=O)([O-])[O-].CO>CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-72f2399edc644c439d5d6ecafa1270b7
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1O.CS(=O)(=O)Cl>>CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1OS(C)(=O)=O
C(C)(=O)OC[C@@H]1[C@H](C[C@@H](O1)N1C(=O)NC(=O)C(C)=C1)O.CS(=O)(=O)Cl.CS(=O)(=O)Cl>>C(C)(=O)OC[C@@H]1[C@H](C[C@@H](O1)N1C(=O)NC(=O)C(C)=C1)OS(=O)(=O)C
[CH3:1][C:2](=[O:3])[O:4][CH2:5][C@H:6]1[O:7][C@@H:8]([n:9]2[cH:10][c:11]([CH3:12])[c:13](=[O:14])[nH:15][c:16]2=[O:17])[CH2:18][C@@H:19]1[OH:20].Cl[S:21]([CH3:22])(=[O:23])=[O:24]>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][C@H:6]1[O:7][C@@H:8]([n:9]2[cH:10][c:11]([CH3:12])[c:13](=[O:14])[nH:15][c:16]2=[O:17])[CH2:18][C@@H:19]1...
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1O.CS(=O)(=O)Cl
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1OS(C)(=O)=O
null
null
N1=CC=CC=C1
Acylation
Formation of Sulfonic Esters
641955d0081c80f158ce2aacd31873a3f3301c87ca0800cf263e288ba8390217
4f9373df8a11470603daf885a5777cebf95940370e32739263d35df0f171a0dd
O=c1ccn([C@H]2CCCO2)c(=O)[nH]1
Cl-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4].[#8:5]-[C:6]-[C:7](-[OH;D1;+0:8])-[C:9]>>[#8:5]-[C:6]-[C:7](-[O;H0;D2;+0:8]-[S;H0;D4;+0:1](-[C;D1;H3:2])(=[O;D1;H0:3])=[O;D1;H0:4])-[C:9]
null
[]
0
CELSIUS
null
null
The 5'-O-acetylthymidine obtained in Example 7 was dissolved in 100 ml of pyridine and cooled to 0° C. Then, 11.57 g (2 equivalents) of methanesulfonyl chloride were added thereto. After these were reacted at 0° C. for 1.5 hours, 5.79 g (one equivalent) of methanesulfonyl chloride were added thereto and reacted at 0° C...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol.Sulfonyl halide
Mesylate
null
null
C1CCOC1.c1cncnc1
HCl
N1=CC=CC=C1
0
null
CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1O.CS(=O)(=O)Cl>N1=CC=CC=C1>CC(=O)OC[C@H]1O[C@@H](n2cc(C)c(=O)[nH]c2=O)C[C@@H]1OS(C)(=O)=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ba6618a5350d412685ae28c1c46959dc
N#CN=C(Oc1ccccc1)Oc1ccccc1.Nc1cncnc1>>N#CN=C(Nc1cncnc1)Oc1ccccc1
C1=CC=C(C=C1)OC(=NC#N)OC2=CC=CC=C2.NC=1C=NC=NC1>>C(#N)N=C(NC=1C=NC=NC1)OC1=CC=CC=C1
c1ccc(O[C:4](=[N:3][C:2]#[N:1])[O:12][c:13]2[cH:14][cH:15][cH:16][cH:17][cH:18]2)cc1.[NH2:5][c:6]1[cH:7][n:8][cH:9][n:10][cH:11]1>>[N:1]#[C:2][N:3]=[C:4]([NH:5][c:6]1[cH:7][n:8][cH:9][n:10][cH:11]1)[O:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1
N#CN=C(Oc1ccccc1)Oc1ccccc1.Nc1cncnc1
N#CN=C(Nc1cncnc1)Oc1ccccc1
null
null
CCOCC
Heteroatom Alkylation and Arylation
OtherReaction
ee096f5ab320ed58f4369523918a4c51313bdefd69ab4de3888cdce5737c1bea
c04464d7d733f4672f5db3386f93d469810e8d1c6e2a36f603b54b46a74b4d93
N=C(Nc1cncnc1)Oc1ccccc1
[N;D1;H0:1]#[C:2]-[#7:3]=[C;H0;D3;+0:4](-O-c1:c:c:c:c:c:1)-[#8:5]-[c:6].[NH2;D1;+0:7]-[c:8]1:[c:9]:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:1>>[N;D1;H0:1]#[C:2]-[#7:3]=[C;H0;D3;+0:4](-[#8:5]-[c:6])-[NH;D2;+0:7]-[c:8]1:[c:9]:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:1
53.9
[{"value": 53.9, "product": "C(#N)N=C(NC=1C=NC=NC1)OC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
DAY
A stirred mixture of diphenyl cyanocarbonimidate (1.05 g, 0.00442 mol), 5-amino-pyrimidine (0.42 g, 0.00442 mol) and Et2O (15 mL) was kept at ambient temperature for 4 days and at reflux for one day. There was little reaction. The solvent was evaporated and the residue was mixed with DME and warmed at 50°-55° for 2 day...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary amine
Ether.Secondary amine
c1ccccc1
null
c1cncnc1.c1ccccc1
HO-
CCOCC
null
96
N#CN=C(Oc1ccccc1)Oc1ccccc1.Nc1cncnc1>CCOCC>N#CN=C(Nc1cncnc1)Oc1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e078ab19abb14e4ab8ca11ba7e1f1bc5
C[C@@H](N)c1ccccc1.N#CN=C(Nc1cncnc1)Oc1ccccc1>>C[C@@H](NC(=NC#N)Nc1cncnc1)c1ccccc1
C(#N)N=C(NC=1C=NC=NC1)OC1=CC=CC=C1.C[C@H](C1=CC=CC=C1)N>>C(#N)N=C(NC=1C=NC=NC1)N[C@H](C)C1=CC=CC=C1
[CH3:1][C@@H:2]([NH2:3])[c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1.c1ccc(O[C:4](=[N:5][C:6]#[N:7])[NH:8][c:9]2[cH:10][n:11][cH:12][n:13][cH:14]2)cc1>>[CH3:1][C@@H:2]([NH:3][C:4](=[N:5][C:6]#[N:7])[NH:8][c:9]1[cH:10][n:11][cH:12][n:13][cH:14]1)[c:15]1[cH:16][cH:17][cH:18][cH:19][cH:20]1
C[C@@H](N)c1ccccc1.N#CN=C(Nc1cncnc1)Oc1ccccc1
C[C@@H](NC(=NC#N)Nc1cncnc1)c1ccccc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
114d8f7243f9e520c2011150952e9826f1217db119c95c007b250beda4b0554b
953ca34981f329c845365ec5b25a3d27fa72aebd3e467f4e6ef8becba38a9d76
N=C(NCc1ccccc1)Nc1cncnc1
[#7;a:1]:[c:2]:[c:3](-[#7:4]-[C;H0;D3;+0:5](-O-c1:c:c:c:c:c:1)=[#7:6]-[C:7]#[N;D1;H0:8]):[c:9]:[#7;a:10].[C;D1;H3:11]-[C:12](-[NH2;D1;+0:13])-[c:14]>>[#7;a:1]:[c:2]:[c:3](-[#7:4]-[C;H0;D3;+0:5](=[#7:6]-[C:7]#[N;D1;H0:8])-[NH;D2;+0:13]-[C:12](-[C;D1;H3:11])-[c:14]):[c:9]:[#7;a:10]
null
[]
null
null
18
HOUR
A stirred mixture of N'-cyano-N-(5-pyrimidyl)-O-phenylisourea (0.5 g, 0.00209 mol), (R)-α-methylbenzylamine (1.0 mL) and DMF (4 mL) was kept, under nitrogen, at ambient temperature for 18 hours and concentrated in vacuo. The residue was allowed to crystallize from EtOAc-tert-butyl methyl ether. The solid was triturated...
10.6084/m9.figshare.5104873.v1
null
Ether.Primary amine
Secondary amine
c1ccccc1
null
c1cncnc1.c1ccccc1
HO-
CN(C)C=O
null
18
C[C@@H](N)c1ccccc1.N#CN=C(Nc1cncnc1)Oc1ccccc1>CN(C)C=O>C[C@@H](NC(=NC#N)Nc1cncnc1)c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-f04f23e0e7f145c18e74c42a102f01f6
COC(C)=O.OCC(CO)CCc1ccc(Br)cc1>>CC(=O)OC[C@@H](CO)CCc1ccc(Br)cc1
BrC1=CC=C(C=C1)CCC(CO)CO.C(C)(=O)OC>>C(C)(=O)OC[C@H](CCC1=CC=C(C=C1)Br)CO
CO[C:2]([CH3:1])=[O:3].[OH:4][CH2:5][CH:6]([CH2:7][OH:8])[CH2:9][CH2:10][c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]1>>[CH3:1][C:2](=[O:3])[O:4][CH2:5][C@@H:6]([CH2:7][OH:8])[CH2:9][CH2:10][c:11]1[cH:12][cH:13][c:14]([Br:15])[cH:16][cH:17]1
COC(C)=O.OCC(CO)CCc1ccc(Br)cc1
CC(=O)OC[C@@H](CO)CCc1ccc(Br)cc1
null
null
null
Acylation
Transesterification
c42e047d71ad2593a6d29093d1fe2ca16ccfd6db7b15eecf1eab340181aef83e
cb08be6428b0a3737df44d00995165c06a05fb7dec4fab744c09315c4f7771d4
c1ccccc1
C-O-[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
null
null
To a solution of 4.6 g of 4-(4-bromophenyl)-2-(hydroxymethyl)butanol in 300 ml of methyl acetate was added 33.1 g of the above PPL preparation. The mixture was stirred while the progress of the reaction was monitored by HPLC method A. When the consumption of diol was complete, the mixture was immediately filtered and t...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary alcohol
Ester
null
null
c1ccccc1
HO-
null
null
null
COC(C)=O.OCC(CO)CCc1ccc(Br)cc1>>CC(=O)OC[C@@H](CO)CCc1ccc(Br)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1445eac5a4014671ac02711e701552ec
COc1ccc(Br)cc1C=O.NO>>COc1ccc(Br)cc1C#N
C(C)(=O)OC(C)=O.BrC1=CC=C(C(C=O)=C1)OC.Cl.NO.C(C)(=O)[O-].[Na+].[OH-].[Na+]>>BrC=1C=CC(=C(C#N)C1)OC
O=[CH:10][c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([Br:7])[cH:8]1.O[NH2:11]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Br:7])[cH:8][c:9]1[C:10]#[N:11]
COc1ccc(Br)cc1C=O.NO
COc1ccc(Br)cc1C#N
null
null
C(C)(=O)O
Miscellaneous
OtherReaction
748a00525e7f639e600a6b1229bb8ce947b6e2e96d815c0b05b54470e6cdbc2a
a27285857ea2428fb666a281ae1a2b961eec077cb33a106e48534c99bfe3d865
c1ccccc1
O-[NH2;D1;+0:1].O=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
100
CELSIUS
1
HOUR
A mixture of 5-Bromo-o-anisaldehyde (6.45 g), hydroxylamine hydrochloride (2.2 g), sodium acetate (4.1 g) and acetic acid (20 mL) was heated at 100° C. with stirring for 1 h. Acetic anhydride was added (20 mL) and the mixture was refluxed for 8 h. The reaction mixture was poured onto ice water and the mixture was made ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
Nitrile
null
null
c1ccccc1
HO-
C(C)(=O)O
100
1
COc1ccc(Br)cc1C=O.NO>C(C)(=O)O>COc1ccc(Br)cc1C#N
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d974bf9235d9408fbea0e1003a2cf886
COc1ccc(Br)cc1C(=N)N.O=C(CO)CO>>COc1ccc(Br)cc1-c1ncc(CO)[nH]1
BrC=1C=CC(=C(C(=N)N)C1)OC.OCC(=O)CO.[Cl-].[NH4+].[OH-].[NH4+]>>BrC=1C=CC(=C(C1)C=1NC(=CN1)CO)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Br:7])[cH:8][c:9]1[C:10](=[NH:11])[NH2:16].O=[C:13]([CH2:12]O)[CH2:14][OH:15]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Br:7])[cH:8][c:9]1-[c:10]1[n:11][cH:12][c:13]([CH2:14][OH:15])[nH:16]1
COc1ccc(Br)cc1C(=N)N.O=C(CO)CO
COc1ccc(Br)cc1-c1ncc(CO)[nH]1
null
null
O1CCCC1
Aromatic Heterocycle Formation
OtherReaction
7040ca240901ea801ff60cc2b70327e852de1f0d8d0e034873a53538d68125d0
099961450c7564589a83083f79d293e700761052a76093ed07ed90267b634558
c1ccc(-c2ncc[nH]2)cc1
O-[CH2;D2;+0:1]-[C;H0;D3;+0:2](=O)-[C:3]-[O;D1;H1:4].[#8:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[C;H0;D3;+0:9](-[NH2;D1;+0:10])=[NH;D1;+0:11]):[c:12]:[c:13]>>[#8:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[c;H0;D3;+0:9]1:[n;H0;D2;+0:11]:[cH;D2;+0:1]:[c;H0;D3;+0:2](-[C:3]-[O;D1;H1:4]):[nH;D2;+0:10]:1):[c:12]:[c:13]
null
[]
90
CELSIUS
null
null
A mixture of 5-Bromo-2-methoxy-benzamidine (1.5 g), 1,3-dihydroxy-acetone dimer (1.0 g), ammonium chloride (1.3 g), tetrahydrofuran (3 mL) and concentrated aqueous ammonium hydroxide (10 mL) was heated at 90° C. for 3 h. The reaction mixture was chilled on ice and the precipitated product was collected and recrystalliz...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary alcohol.Primary amine
null
null
c1c[nH]cn1
c1ccccc1.c1c[nH]cn1
HO-
O1CCCC1
90
null
COc1ccc(Br)cc1C(=N)N.O=C(CO)CO>O1CCCC1>COc1ccc(Br)cc1-c1ncc(CO)[nH]1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-560b22e6b12f490aa00ae31becc38836
O=S(Cl)Cl.OCc1ccc(Cl)nc1>>ClCc1ccc(Cl)nc1
ClC1=NC=C(C=C1)CO.S(=O)(Cl)Cl>>ClC1=NC=C(C=C1)CCl
O=S(Cl)[Cl:1].O[CH2:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[n:8][cH:9]1>>[Cl:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[n:8][cH:9]1
O=S(Cl)Cl.OCc1ccc(Cl)nc1
ClCc1ccc(Cl)nc1
null
null
ClCCCl
Functional Group Interconversion
Alcohol to chloride_SOCl2
bb752b9027dc4488ba075e5955118a819f80cabd751a7497b67c2eeb1db6b071
cbf41c7cf9fe6b47a243b1674d74ed5bf46a151f7f3a71d206e23176e158facf
c1ccncc1
Cl-S(=O)-[Cl;H0;D1;+0:1].O-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]>>[Cl;H0;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]:[#7;a:6]:[c:7]
95.7
[{"value": 95.7, "product": "ClC1=NC=C(C=C1)CCl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
A mixture of 70.3 g of 2-chloro-5-(hydroxymethyl) pyridine and 50 ml of 1,2-dichloroethane was dropwise added to a mixture of 87.4 g of thionyl chloride and 100 ml of 1,2-dichloroethane during 30 minutes in a water bath of 5°-20° C. The mixture was stirred for an hour and a half at room temperature and for 4 hours and ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Primary halide
null
null
c1ccncc1
HCl
ClCCCl
null
4
O=S(Cl)Cl.OCc1ccc(Cl)nc1>ClCCCl>ClCc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-62a17c750f504895890fca3760e1030c
ClCc1ccc(Cl)nc1.N>>NCc1ccc(Cl)nc1
[OH-].[Na+].ClC1=NC=C(C=C1)CCl.O.N>>NCC=1C=CC(=NC1)Cl
Cl[CH2:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[n:8][cH:9]1.[NH3:1]>>[NH2:1][CH2:2][c:3]1[cH:4][cH:5][c:6]([Cl:7])[n:8][cH:9]1
ClCc1ccc(Cl)nc1.N
NCc1ccc(Cl)nc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
141e57e7b467ef1af7390eea74d28aab60295f9a2146f5e9c32bccbe8d06fe6f
14467bdca40cd5f74ac0c15917a737e6b818cd36a46b0668375c9383066b6e0b
c1ccncc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[NH3;D0;+0:7]>>[NH2;D1;+0:7]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
58.1
[{"value": 58.1, "product": "NCC=1C=CC(=NC1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
2
HOUR
A mixture of 14.99 g of 2-chloro-5-(chloromethyl) pyridine, 63.01 g of 25% ammonia water and 60 ml of acetonitrile in a stainless steel autoclave was stirred for 2 hours in an oil bath of 80° C. After adding 12.3 g of 30% sodium hydroxide aqueous solution, the reaction mixture was concentrated. The residue to which 200...
10.6084/m9.figshare.5104873.v1
null
Primary halide
Primary amine
null
null
c1ccncc1
HCl
C(C)#N
80
2
ClCc1ccc(Cl)nc1.N>C(C)#N>NCc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-15349f90d5234b6aaef6d84c3387a9b8
CN.ClCc1ccc(Cl)nc1>>CNCc1ccc(Cl)nc1
ClC1=NC=C(C=C1)CCl.CN>>ClC1=NC=C(C=C1)CNC
[CH3:1][NH2:2].Cl[CH2:3][c:4]1[cH:5][cH:6][c:7]([Cl:8])[n:9][cH:10]1>>[CH3:1][NH:2][CH2:3][c:4]1[cH:5][cH:6][c:7]([Cl:8])[n:9][cH:10]1
CN.ClCc1ccc(Cl)nc1
CNCc1ccc(Cl)nc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
N-alkylation of primary amines with alkyl halides
fc19a1445ff204e66e51735d0191465bda3c6691fd233624a54742c9d4828411
0b1d32f56ad00f1e5bdae9390f9227bbea012fa2f8203aac34726b8a6761cc7c
c1ccncc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C;D1;H3:7]-[NH;D2;+0:8]-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6]
60.3
[{"value": 60.3, "product": "ClC1=NC=C(C=C1)CNC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 15.05 g of 2-chloro-5-(chloromethyl) pyridine and 50 ml of acetonitrile was dropwise added to a mixture of 36 g of 40% methylamine aqueous solution and 200 ml of acetonitrile during an hour at room temperature and stirred for an hour and a half. The reaction mixture was concentrated. The resulting residue ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary amine
Secondary amine
null
null
c1ccncc1
HCl
C(C)#N
null
null
CN.ClCc1ccc(Cl)nc1>C(C)#N>CNCc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ddec34ddcf93426ea32b4d8fd7bea2af
CN=C=S.Nc1ccc(Cl)nc1>>CNC(=S)Nc1ccc(Cl)nc1
ClC1=NC=C(C=C1)N.CN=C=S.CN=C=S>>ClC1=CC=C(C=N1)NC(=S)NC
[CH3:1][N:2]=[C:3]=[S:4].[NH2:5][c:6]1[cH:7][cH:8][c:9]([Cl:10])[n:11][cH:12]1>>[CH3:1][NH:2][C:3](=[S:4])[NH:5][c:6]1[cH:7][cH:8][c:9]([Cl:10])[n:11][cH:12]1
CN=C=S.Nc1ccc(Cl)nc1
CNC(=S)Nc1ccc(Cl)nc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
thiourea
9037f368cdf8e91fcd9f93f4d9cf27991f85fa921c9d19c7875d3a77561f439b
0fbf3d6c8cd704ac451c2cf111f32090de5e76a9d41cce326e212c758f4ed46f
c1ccncc1
[C;D1;H3:1]-[N;H0;D2;+0:2]=[C;H0;D2;+0:3]=[S;D1;H0:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]:[#7;a:9]:[c:10]>>[C;D1;H3:1]-[NH;D2;+0:2]-[C;H0;D3;+0:3](=[S;D1;H0:4])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]:[#7;a:9]:[c:10]
70.6
[{"value": 70.6, "product": "ClC1=CC=C(C=N1)NC(=S)NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 4.07 g of 2-chloro-5-aminopyridine, 2.55 g of methyl isothiocyanate and 30 ml of acetonitrile was refluxed for 13.5 hours, to which 0.70 g of additional methyl isothiocyanate was added and the mixture was refluxed for 3.5 hours. The reaction mixture was concentrated, and the residue was purified by a colum...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Isothiocyanate
Thiourea
null
null
c1ccncc1
null
C(C)#N
null
null
CN=C=S.Nc1ccc(Cl)nc1>C(C)#N>CNC(=S)Nc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0ae21637521349e3a5ce4e7dee9dae97
CCNCC.CSC(=N)N[N+](=O)[O-]>>CCN(CC)C(=N)N[N+](=O)[O-]
CSC(N[N+](=O)[O-])=N.C(C)NCC>>C(C)N(C(=N)N[N+](=O)[O-])CC
[CH3:1][CH2:2][NH:3][CH2:4][CH3:5].CS[C:6](=[NH:7])[NH:8][N+:9](=[O:10])[O-:11]>>[CH3:1][CH2:2][N:3]([CH2:4][CH3:5])[C:6](=[NH:7])[NH:8][N+:9](=[O:10])[O-:11]
CCNCC.CSC(=N)N[N+](=O)[O-]
CCN(CC)C(=N)N[N+](=O)[O-]
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
05b64877b6cb13a4648efb144268a1124b146a9cb0b909480944b9bd8a435a49
f5aa33108984aad43441754644c214239e577e2035dc027b4aa13ab85821a21b
null
C-S-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6].[C;D1;H3:7]-[C:8]-[NH;D2;+0:9]-[C:10]-[C;D1;H3:11]>>[C;D1;H3:7]-[C:8]-[N;H0;D3;+0:9](-[C:10]-[C;D1;H3:11])-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6]
53.1
[{"value": 53.1, "product": "C(C)N(C(=N)N[N+](=O)[O-])CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
6
HOUR
To a mixture of 1.35 g of S-methyl-N-nitroisothiourea and 5 ml of acetonitrile was added 0.88 g of diethylamine, followed by stirring for 6 hours in an oil bath of 60° C. The reaction mixture was concentrated and the residue was purified by a column chromatography [developing solvent: dichloromethanemethanol (20:1)] to...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Monosulfide
Tertiary amine
null
null
null
Other
C(C)#N
60
6
CCNCC.CSC(=N)N[N+](=O)[O-]>C(C)#N>CCN(CC)C(=N)N[N+](=O)[O-]
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-7b39bae98337414e9faa77d40fa49602
C1CCNC1.CSC(=N)N[N+](=O)[O-]>>N=C(N[N+](=O)[O-])N1CCCC1
CSC(N[N+](=O)[O-])=N.N1CCCC1>>[N+](=O)([O-])NC(=N)N1CCCC1
[NH:7]1[CH2:8][CH2:9][CH2:10][CH2:11]1.CS[C:2](=[NH:1])[NH:3][N+:4](=[O:5])[O-:6]>>[NH:1]=[C:2]([NH:3][N+:4](=[O:5])[O-:6])[N:7]1[CH2:8][CH2:9][CH2:10][CH2:11]1
C1CCNC1.CSC(=N)N[N+](=O)[O-]
N=C(N[N+](=O)[O-])N1CCCC1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
868057ed7bfa967ecc158180c4e484530f29269be5b11d1bfeff00362dda8c2e
f5aa33108984aad43441754644c214239e577e2035dc027b4aa13ab85821a21b
C1CCNC1
C-S-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6].[C:7]1-[C:8]-[NH;D2;+0:9]-[C:10]-[C:11]-1>>[N;D1;H1:2]=[C;H0;D3;+0:1](-[#7:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6])-[N;H0;D3;+0:9]1-[C:8]-[C:7]-[C:11]-[C:10]-1
93.1
[{"value": 93.1, "product": "[N+](=O)([O-])NC(=N)N1CCCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a mixture of 1.0 g of S-methyl-N-nitroisothiourea and 15 ml of acetonitrile was dropwise added 0.61 g of pyrrolidine within 2 minutes, followed by stirring for 30 minutes. The reaction mixture was concentrated. The resulting precipitate was washed with ethyl ether to afford 1.09 g of 1-(N-nitroamidino)pyrrolidine as...
10.6084/m9.figshare.5104873.v1
null
Secondary amine.Monosulfide
Tertiary amine
C1CCNC1
C1CC[NH]C1
C1CC[NH]C1
Other
C(C)#N
null
0.5
C1CCNC1.CSC(=N)N[N+](=O)[O-]>C(C)#N>N=C(N[N+](=O)[O-])N1CCCC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-202a43352c1f4b68988506e8d117a5f3
CC(=O)OC(C)=O.CSC(=N)N[N+](=O)[O-]>>CSC(=N[N+](=O)[O-])NC(C)=O
CSC(N[N+](=O)[O-])=N.C(C)(=O)OC(C)=O>>C(C)(=O)NC(SC)=N[N+](=O)[O-]
CC(=O)O[C:9]([CH3:10])=[O:11].[CH3:1][S:2][C:3]([NH:4][N+:5](=[O:6])[O-:7])=[NH:8]>>[CH3:1][S:2][C:3](=[N:4][N+:5](=[O:6])[O-:7])[NH:8][C:9]([CH3:10])=[O:11]
CC(=O)OC(C)=O.CSC(=N)N[N+](=O)[O-]
CSC(=N[N+](=O)[O-])NC(C)=O
null
null
N1=CC=CC=C1
Acylation
OtherReaction
5179bd03f895b7267efad9d9919c77d0bc7bead4953793964c6224650ae47b34
ee9858b53576953e7a3de0544c9c100a5576f5cd0c0f2d39deb4c9decc8e363a
null
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[C;D1;H3:4]-[#16:5]-[C;H0;D3;+0:6](=[NH;D1;+0:7])-[NH;D2;+0:8]-[#7;+:9](-[O;-;D1;H0:10])=[O;D1;H0:11]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[NH;D2;+0:7]-[C;H0;D3;+0:6](-[#16:5]-[C;D1;H3:4])=[N;H0;D2;+0:8]-[#7;+:9](-[O;-;D1;H0:10])=[O;D1;H0:11]
77.8
[{"value": 77.8, "product": "C(C)(=O)NC(SC)=N[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a mixture of 5.0 g of S-methyl-N-nitroisothiourea and 25 ml of pyridine was dropwise added 11.3 g of acetic anhydride at room temperature, taking for 10 minutes, followed by stirring for 5 hours at the same temperature. The reaction mixture was concentrated, and the residue was poured into 50 ml of 2N-hydrochloric a...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Anhydride.Monosulfide
Hydrazone.Secondary amide
null
null
null
HO-
N1=CC=CC=C1
null
0.166667
CC(=O)OC(C)=O.CSC(=N)N[N+](=O)[O-]>N1=CC=CC=C1>CSC(=N[N+](=O)[O-])NC(C)=O
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e77115f6fff944f5b5d1ed887385f92e
CCOC(=O)C(Cl)C=O.NC(=S)C(F)(F)F>>CCOC(=O)c1cnc(C(F)(F)F)s1
FC(C(=S)N)(F)F.ClC(C(=O)OCC)C=O>>FC(C=1SC(=CN1)C(=O)OCC)(F)F
O=[CH:7][CH:6](Cl)[C:4]([O:3][CH2:2][CH3:1])=[O:5].[NH2:8][C:9]([C:10]([F:11])([F:12])[F:13])=[S:14]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[cH:7][n:8][c:9]([C:10]([F:11])([F:12])[F:13])[s:14]1
CCOC(=O)C(Cl)C=O.NC(=S)C(F)(F)F
CCOC(=O)c1cnc(C(F)(F)F)s1
null
null
ClCCl
Aromatic Heterocycle Formation
OtherReaction
ca1a491634351402ba53e022aaddc0a4c7ec0639045153b7668e78d316c6754f
b332eb5ea501618d8dbac38c7e3242fcefa783e31f17b6ca5d4aaeb74530fc69
c1cscn1
Cl-[CH;D3;+0:1](-[CH;D2;+0:2]=O)-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6].[F;D1;H0:7]-[C:8](-[F;D1;H0:9])(-[F;D1;H0:10])-[C;H0;D3;+0:11](-[NH2;D1;+0:12])=[S;H0;D1;+0:13]>>[C:6]-[#8:5]-[C:3](=[O;D1;H0:4])-[c;H0;D3;+0:1]1:[cH;D2;+0:2]:[n;H0;D2;+0:12]:[c;H0;D3;+0:11](-[C:8](-[F;D1;H0:7])(-[F;D1;H0:9])-[F;D1;H0:10]):[s;H0;D2;+0:13...
24.7
[{"value": 24.7, "product": "FC(C=1SC(=CN1)C(=O)OCC)(F)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
30
MINUTE
A mixture of 11.22 g of 2,2,2,-trifluorothioacetamide and 10.14 g of ethyl 2-chloro-2-formylacetate was stirred for 30 minutes in an oil bath of 70° C. and then for 1.5 hours in an oil bath of 100° C., to which 100 ml of dichloromethane were added. After removing an insoluble substance, the mixture was concentrated and...
10.6084/m9.figshare.5104873.v1
null
Secondary halide.Aldehyde.Ester.Thioamide
Ester
null
c1cscn1
c1cscn1
HCl
ClCCl
70
0.5
CCOC(=O)C(Cl)C=O.NC(=S)C(F)(F)F>ClCCl>CCOC(=O)c1cnc(C(F)(F)F)s1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-ea67113aecf847ec8fb13bda32202f05
CCN(Cc1ccc(Cl)nc1)C(=NC#N)SC.CN>>CCN(Cc1ccc(Cl)nc1)C(=NC#N)NC
ClC1=CC=C(C=N1)CN(C(SC)=NC#N)CC.CN>>ClC1=CC=C(C=N1)CN(C(=NC#N)NC)CC
CS[C:12]([N:3]([CH2:2][CH3:1])[CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[n:10][cH:11]1)=[N:13][C:14]#[N:15].[NH2:16][CH3:17]>>[CH3:1][CH2:2][N:3]([CH2:4][c:5]1[cH:6][cH:7][c:8]([Cl:9])[n:10][cH:11]1)[C:12](=[N:13][C:14]#[N:15])[NH:16][CH3:17]
CCN(Cc1ccc(Cl)nc1)C(=NC#N)SC.CN
CCN(Cc1ccc(Cl)nc1)C(=NC#N)NC
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
2ebe33ae3b7bb48bd968f9b830d6d3b488b85670dea18c3fe37a1f418e787d67
88e0224d19b2dce8f9987d52554afb32090d36ff7ee19e89dc5bf66d30974ec4
c1ccncc1
C-S-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[#7:5](-[C:6])-[C:7].[C;D1;H3:8]-[NH2;D1;+0:9]>>[C:6]-[#7:5](-[C:7])-[C;H0;D3;+0:1](=[#7:2]-[C:3]#[N;D1;H0:4])-[NH;D2;+0:9]-[C;D1;H3:8]
81.4
[{"value": 81.4, "product": "ClC1=CC=C(C=N1)CN(C(=NC#N)NC)CC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a mixture of 0.42 g of 1-(6-chloro-3-pyridylmethyl)-3-cyano-1-ethyl-2-methylisothiourea and 5 ml of acetonitrile was added each 0.5 g of 40% methylamine aqueous solution at an hour interval in total six time (3.0 g), while refluxing and stirring. The reaction mixture was stirred for 6 hours in total. Then, the mixtu...
10.6084/m9.figshare.5104873.v1
null
Primary amine.Monosulfide
Secondary amine
null
null
c1ccncc1
Other
C(C)#N
null
null
CCN(Cc1ccc(Cl)nc1)C(=NC#N)SC.CN>C(C)#N>CCN(Cc1ccc(Cl)nc1)C(=NC#N)NC
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-e223f8a6637044d994743a5abd5433cf
CN(C)C(=N)N[N+](=O)[O-].ClCc1ccc(Cl)nc1>>CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
[H-].[Na+].CN(C(=N)N[N+](=O)[O-])C.ClC1=NC=C(C=C1)CCl>>ClC1=CC=C(C=N1)CNC(=N[N+](=O)[O-])N(C)C
[CH3:1][N:2]([CH3:3])[C:4]([NH:5][N+:6](=[O:7])[O-:8])=[NH:9].Cl[CH2:10][c:11]1[cH:12][cH:13][c:14]([Cl:15])[n:16][cH:17]1>>[CH3:1][N:2]([CH3:3])[C:4](=[N:5][N+:6](=[O:7])[O-:8])[NH:9][CH2:10][c:11]1[cH:12][cH:13][c:14]([Cl:15])[n:16][cH:17]1
CN(C)C(=N)N[N+](=O)[O-].ClCc1ccc(Cl)nc1
CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
null
null
CN(C)C=O
Protection
OtherReaction
6bc260a19edaf0a9ae100808188306f3bdd7a4767e9712a41beac901d2272dbe
ee9f583c221e42a578248439e705971d77c8a525da3f66f469ff1a1aba186bf7
c1ccncc1
Cl-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]:[#7;a:5]:[c:6].[C;D1;H3:7]-[#7:8](-[C;D1;H3:9])-[C;H0;D3;+0:10](=[NH;D1;+0:11])-[NH;D2;+0:12]-[#7;+:13](-[O;-;D1;H0:14])=[O;D1;H0:15]>>[C;D1;H3:7]-[#7:8](-[C;D1;H3:9])-[C;H0;D3;+0:10](=[N;H0;D2;+0:12]-[#7;+:13](-[O;-;D1;H0:14])=[O;D1;H0:15])-[NH;D2;+0:11]-[CH2;D2;+0:1]-[c:2](:[c:3])...
31.9
[{"value": 31.9, "product": "ClC1=CC=C(C=N1)CNC(=N[N+](=O)[O-])N(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a suspension of 0.44 g of 60% sodium hydride (in mineral oil) in 10 ml of DMF was added 1.32 g of N,N-dimethyl-N'-nitroguanidine during 20 minutes at room temperature. After stirring for 10 minutes, 1.62 g of 2-chloro-5-(chloromethyl)pyridine was added to the mixture in 5 minutes, and stirred for 2 hours at room tem...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Primary halide
Hydrazone.Secondary amine
null
null
c1ccncc1
HCl
CN(C)C=O
null
0.166667
CN(C)C(=N)N[N+](=O)[O-].ClCc1ccc(Cl)nc1>CN(C)C=O>CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-a0d445180fdc49e09290c6b0997b3fc5
CNC(=N[N+](=O)[O-])SC.NCc1ccc(Cl)nc1>>CNC(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
CNC(SC)=N[N+](=O)[O-].NCC=1C=CC(=NC1)Cl>>ClC1=CC=C(C=N1)CNC(=N[N+](=O)[O-])NC
CS[C:3]([NH:2][CH3:1])=[N:4][N+:5](=[O:6])[O-:7].[NH2:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([Cl:14])[n:15][cH:16]1>>[CH3:1][NH:2][C:3](=[N:4][N+:5](=[O:6])[O-:7])[NH:8][CH2:9][c:10]1[cH:11][cH:12][c:13]([Cl:14])[n:15][cH:16]1
CNC(=N[N+](=O)[O-])SC.NCc1ccc(Cl)nc1
CNC(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
883fee3f84362c063113a06e86cdc3a3bf94029e9de373b9cf505859a3b7d61a
07cba6ae0650a80cbffb2d3f121f3eee9c0a2be72294ae9df786d5ac7452446b
c1ccncc1
C-S-[C;H0;D3;+0:1](-[#7:2]-[C;D1;H3:3])=[#7:4]-[#7;+:5](-[O;-;D1;H0:6])=[O;D1;H0:7].[#7;a:8]:[c:9]:[c:10]-[C:11]-[NH2;D1;+0:12]>>[#7;a:8]:[c:9]:[c:10]-[C:11]-[NH;D2;+0:12]-[C;H0;D3;+0:1](-[#7:2]-[C;D1;H3:3])=[#7:4]-[#7;+:5](-[O;-;D1;H0:6])=[O;D1;H0:7]
34
[{"value": 34.0, "product": "ClC1=CC=C(C=N1)CNC(=N[N+](=O)[O-])NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 0.45 g of 1,2-dimethyl-3-nitroisothiourea, 0.43 g of 5-(aminomethyl)-2-chloropyridine and 25 ml of ethanol was refluxed for 6 hours and concentrated. The residue was purified by a column chromatography [developing solvent: chloroform-ethanol (5:1)] to afford 0.25 g of 1-(6-chloro-3-pyridylmethyl)-3-methyl-...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Primary amine.Monosulfide
Hydrazone.Secondary amine
null
null
c1ccncc1
Other
C(C)O
null
null
CNC(=N[N+](=O)[O-])SC.NCc1ccc(Cl)nc1>C(C)O>CNC(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-eb6b1e439c704066992f2dc01030ffe1
CNCc1ccc(Cl)nc1.CSC(=N)N[N+](=O)[O-]>>CN(Cc1ccc(Cl)nc1)C(N)=N[N+](=O)[O-]
CSC(N[N+](=O)[O-])=N.ClC1=NC=C(C=C1)CNC>>ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])N)C
[CH3:1][NH:2][CH2:3][c:4]1[cH:5][cH:6][c:7]([Cl:8])[n:9][cH:10]1.CS[C:11](=[NH:12])[NH:13][N+:14](=[O:15])[O-:16]>>[CH3:1][N:2]([CH2:3][c:4]1[cH:5][cH:6][c:7]([Cl:8])[n:9][cH:10]1)[C:11]([NH2:12])=[N:13][N+:14](=[O:15])[O-:16]
CNCc1ccc(Cl)nc1.CSC(=N)N[N+](=O)[O-]
CN(Cc1ccc(Cl)nc1)C(N)=N[N+](=O)[O-]
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
8492a5db8ba38868aaf8f542781290a626677d540b1f2ec0ede58678eb181444
a6d74864a38e00e28e7bd6e7158dd0ac81d24c0ac9fdb6de46f9333a7dc0e609
c1ccncc1
C-S-[C;H0;D3;+0:1](=[NH;D1;+0:2])-[NH;D2;+0:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6].[#7;a:7]:[c:8]:[c:9]-[C:10]-[NH;D2;+0:11]-[C;D1;H3:12]>>[#7;a:7]:[c:8]:[c:9]-[C:10]-[N;H0;D3;+0:11](-[C;D1;H3:12])-[C;H0;D3;+0:1](-[NH2;D1;+0:2])=[N;H0;D2;+0:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6]
31.2
[{"value": 31.2, "product": "ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])N)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 0.676 g of S-methyl-N-nitroisothiourea, 0.783 g of 2-chloro-5-(methylaminomethyl)pyridine and 6 ml of acetonitrile was refluxed for 17 hours, and concentrated. The residue was recrystallized from ethanol to obtain 0.38 g of 1-(6-chloro-3-pyridylmethyl)-1-methyl-2-nitroguanidine (Compound No. 7). Conditions...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Secondary amine.Monosulfide
Hydrazone.Primary amine.Tertiary amine
null
null
c1ccncc1
Other
C(C)#N
null
null
CNCc1ccc(Cl)nc1.CSC(=N)N[N+](=O)[O-]>C(C)#N>CN(Cc1ccc(Cl)nc1)C(N)=N[N+](=O)[O-]
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-cfb1593aec87497ca8ab97928a86ad43
CN.CSC(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1>>CNC(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
ClC1=CC=C(C=N1)CN(C(SC)=N[N+](=O)[O-])C.CN>>ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])NC)C
[CH3:1][NH2:2].CS[C:3](=[N:4][N+:5](=[O:6])[O-:7])[N:8]([CH3:9])[CH2:10][c:11]1[cH:12][cH:13][c:14]([Cl:15])[n:16][cH:17]1>>[CH3:1][NH:2][C:3](=[N:4][N+:5](=[O:6])[O-:7])[N:8]([CH3:9])[CH2:10][c:11]1[cH:12][cH:13][c:14]([Cl:15])[n:16][cH:17]1
CN.CSC(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
CNC(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
883fee3f84362c063113a06e86cdc3a3bf94029e9de373b9cf505859a3b7d61a
07cba6ae0650a80cbffb2d3f121f3eee9c0a2be72294ae9df786d5ac7452446b
c1ccncc1
C-S-[C;H0;D3;+0:1](=[#7:2]-[#7;+:3](-[O;-;D1;H0:4])=[O;D1;H0:5])-[#7:6](-[C:7])-[C;D1;H3:8].[C;D1;H3:9]-[NH2;D1;+0:10]>>[C:7]-[#7:6](-[C;D1;H3:8])-[C;H0;D3;+0:1](=[#7:2]-[#7;+:3](-[O;-;D1;H0:4])=[O;D1;H0:5])-[NH;D2;+0:10]-[C;D1;H3:9]
72.8
[{"value": 72.8, "product": "ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])NC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
70
CELSIUS
2
HOUR
A mixture of 0.82 g of 1-(6-chloro-3-pyridyl-methyl)-1,2-dimethyl-3-nitroisothiourea, 0.464 g of 40% methylamine aqueous solution and 10 ml of acetonitrile was stirred for 2 hours at 70° C., and concentrated. The residue was purified by a column chromatography developing solution: dichloromethane-methanol [10:1]) to af...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Primary amine.Monosulfide
Hydrazone.Secondary amine
null
null
c1ccncc1
Other
C(C)#N
70
2
CN.CSC(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1>C(C)#N>CNC(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1bca00ba48324653a225f7149bb02d40
N=C(N)N[N+](=O)[O-].NCc1cccnc1>>N=C(NCc1cccnc1)N[N+](=O)[O-]
[N+](=O)([O-])NC(=N)N.NCC=1C=NC=CC1>>[N+](=O)([O-])NC(=N)NCC=1C=NC=CC1
N[C:2](=[NH:1])[NH:11][N+:12](=[O:13])[O-:14].[NH2:3][CH2:4][c:5]1[cH:6][cH:7][cH:8][n:9][cH:10]1>>[NH:1]=[C:2]([NH:3][CH2:4][c:5]1[cH:6][cH:7][cH:8][n:9][cH:10]1)[NH:11][N+:12](=[O:13])[O-:14]
N=C(N)N[N+](=O)[O-].NCc1cccnc1
N=C(NCc1cccnc1)N[N+](=O)[O-]
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
3a57d6854f77082d71e7a55c408a198c46ae4aa81ffd8dae0cb36847fdc88419
d3d09bdf4511175432d42d1477b84cc1bf1a82e217a37c22fa170c7e0beabdc1
c1ccncc1
N-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6].[#7;a:7]:[c:8]:[c:9]-[C:10]-[NH2;D1;+0:11]>>[#7;a:7]:[c:8]:[c:9]-[C:10]-[NH;D2;+0:11]-[C;H0;D3;+0:1](=[N;D1;H1:2])-[#7:3]-[#7;+:4](-[O;-;D1;H0:5])=[O;D1;H0:6]
48.3
[{"value": 48.3, "product": "[N+](=O)([O-])NC(=N)NCC=1C=NC=CC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
A mixture of 0.53 g of nitroguanidine, 0.61 g of 3-(aminomethyl)pyridine and 10 ml of water was stirred for 1.5 hours at 70°-80° C. and allowed to stand over night at room temperature. The precipitate collected by filtration was washed with ethanol to obtain 0.48 g of N-nitro-N'-(3-pyridylmethyl)guanidine (Compound No....
10.6084/m9.figshare.5104873.v1
null
Primary amine.Primary amine
Secondary amine
null
null
c1ccncc1
Other
O
null
1.5
N=C(N)N[N+](=O)[O-].NCc1cccnc1>O>N=C(NCc1cccnc1)N[N+](=O)[O-]
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-bdd54f199ffc42b194e4d4d34c788ac0
CI.CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1>>CN(C)C(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
C(C)(=O)O.IC.ClC1=CC=C(C=N1)CNC(=N[N+](=O)[O-])N(C)C.[H-].[Na+]>>ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])N(C)C)C
I[CH3:10].[CH3:1][N:2]([CH3:3])[C:4](=[N:5][N+:6](=[O:7])[O-:8])[NH:9][CH2:11][c:12]1[cH:13][cH:14][c:15]([Cl:16])[n:17][cH:18]1>>[CH3:1][N:2]([CH3:3])[C:4](=[N:5][N+:6](=[O:7])[O-:8])[N:9]([CH3:10])[CH2:11][c:12]1[cH:13][cH:14][c:15]([Cl:16])[n:17][cH:18]1
CI.CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
CN(C)C(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
e1587a52a1bca6a80c6048d43276d8bccf8d3e94e692e6b210e5fd3b22494187
7cc25fba33369069673bac5bd8fc404dc064da8d6c8cf4a77f21f4df0a617fe3
c1ccncc1
I-[CH3;D1;+0:1].[#7:2]-[C:3](=[#7:4]-[#7;+:5])-[NH;D2;+0:6]-[C:7]-[c:8]:[c:9]:[#7;a:10]>>[#7:2]-[C:3](=[#7:4]-[#7;+:5])-[N;H0;D3;+0:6](-[CH3;D1;+0:1])-[C:7]-[c:8]:[c:9]:[#7;a:10]
null
[]
null
null
30
MINUTE
To a mixture of 0.24 g of 1-(6-chloro-3-pyridylmethyl)-3,3-dimethyl-2-nitroguanidine (Compound No. 6) and 6 ml of dry tetrahydrofuran (THF) was added 0.045 g of 60% sodium hydride (in mineral oil) at room temperature, followed by stirring for 30 minutes. A solution of 0.16 g of iodomethane in 1 ml of THF was added to t...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Tertiary amine
null
null
c1ccncc1
HI
O1CCCC1
null
0.5
CI.CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1>O1CCCC1>CN(C)C(=N[N+](=O)[O-])N(C)Cc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-00bb20223361438ca1a237b149f0cebc
CC(=O)OC=O.CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1>>CN(C)C(=N[N+](=O)[O-])N(C=O)Cc1ccc(Cl)nc1
[H-].[Na+].ClC1=CC=C(C=N1)CNC(=N[N+](=O)[O-])N(C)C.C(=O)OC(C)=O>>ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])N(C)C)C=O
CC(=O)O[CH:10]=[O:11].[CH3:1][N:2]([CH3:3])[C:4](=[N:5][N+:6](=[O:7])[O-:8])[NH:9][CH2:12][c:13]1[cH:14][cH:15][c:16]([Cl:17])[n:18][cH:19]1>>[CH3:1][N:2]([CH3:3])[C:4](=[N:5][N+:6](=[O:7])[O-:8])[N:9]([CH:10]=[O:11])[CH2:12][c:13]1[cH:14][cH:15][c:16]([Cl:17])[n:18][cH:19]1
CC(=O)OC=O.CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
CN(C)C(=N[N+](=O)[O-])N(C=O)Cc1ccc(Cl)nc1
null
null
C1CCOC1
Acylation
OtherReaction
d178cf3b7716e98c877fb8e7fd543bf80bf7ca766a3397de1d00b85a8dc4cbce
a915e3923d0587efcb1952fd34158dabaf6121028d5282bdf34c96ebf77c7ff6
c1ccncc1
C-C(=O)-O-[CH;D2;+0:1]=[O;D1;H0:2].[#7:3]-[C:4](=[#7:5]-[#7;+:6])-[NH;D2;+0:7]-[C:8]-[c:9]:[c:10]:[#7;a:11]>>[#7:3]-[C:4](=[#7:5]-[#7;+:6])-[N;H0;D3;+0:7](-[C:8]-[c:9]:[c:10]:[#7;a:11])-[CH;D2;+0:1]=[O;D1;H0:2]
34.7
[{"value": 34.7, "product": "ClC1=CC=C(C=N1)CN(C(=N[N+](=O)[O-])N(C)C)C=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a mixture of 0.26 g of 1-(6-chloro-3-pyridylmethyl)-3,3-dimethyl-2-nitroguanidine (Compound No. 6) and 3 ml of dry THF was added 0.08 g of 60% sodium hydride (in mineral oil) in a water bath of 20° C., followed by stirring for 30 minutes. A solution of 0.26 g of acetic formic anhydride in 0.5 ml of THF was added to ...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Ester.Secondary amine
Tertiary amide
null
null
c1ccncc1
HO-
C1CCOC1
null
0.5
CC(=O)OC=O.CN(C)C(=N[N+](=O)[O-])NCc1ccc(Cl)nc1>C1CCOC1>CN(C)C(=N[N+](=O)[O-])N(C=O)Cc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-deb5e3067b824df78fe41cdb691c4394
CNC(=S)Nc1ccc(Cl)nc1.N#CN>>CNC(=NC#N)Nc1ccc(Cl)nc1
ClC1=CC=C(C=N1)NC(=S)NC.N#CN.C1(CCCCC1)N=C=NC1CCCCC1>>ClC1=CC=C(C=N1)NC(=NC#N)NC
S=[C:3]([NH:2][CH3:1])[NH:7][c:8]1[cH:9][cH:10][c:11]([Cl:12])[n:13][cH:14]1.[NH2:4][C:5]#[N:6]>>[CH3:1][NH:2][C:3](=[N:4][C:5]#[N:6])[NH:7][c:8]1[cH:9][cH:10][c:11]([Cl:12])[n:13][cH:14]1
CNC(=S)Nc1ccc(Cl)nc1.N#CN
CNC(=NC#N)Nc1ccc(Cl)nc1
null
C(C)N(C(C)C)C(C)C
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
a1eed482de64f210d0aa14250aff2e95896d7c125f5ef11d8db9968ccb473ed2
42f73345310a096555cb36ab9248c959f01ac661f032df704842b690aa63e637
c1ccncc1
S=[C;H0;D3;+0:1](-[#7:2]-[C;D1;H3:3])-[#7:4]-[c:5]:[c:6]:[#7;a:7].[N;D1;H0:8]#[C:9]-[NH2;D1;+0:10]>>[#7;a:7]:[c:6]:[c:5]-[#7:4]-[C;H0;D3;+0:1](-[#7:2]-[C;D1;H3:3])=[N;H0;D2;+0:10]-[C:9]#[N;D1;H0:8]
29
[{"value": 29.0, "product": "ClC1=CC=C(C=N1)NC(=NC#N)NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
34
HOUR
A mixture of 1.03 g of 1-(6-chloro-3-pyridyl)-3-methylthiourea, 0.32 g of cyanamide, 1.58 g of dicyclohexylcarbodiimide, 3 drops of ethyl diisopropylamine and 10 ml of acetonitrile was stirred for 34 hours at room temperature and filtered to collect an insoluble substance. The insoluble substance was recrystallized fro...
10.6084/m9.figshare.5104873.v1
null
Cyanamide.Thiourea
null
null
null
c1ccncc1
Other
C(C)N(C(C)C)C(C)C.C(C)#N
null
34
CNC(=S)Nc1ccc(Cl)nc1.N#CN>C(C)N(C(C)C)C(C)C.C(C)#N>CNC(=NC#N)Nc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d848d8ca30a34c3cba54395a638315e6
CNC(=N[N+](=O)[O-])SC.NCc1cnc(Br)s1>>CNC(=N[N+](=O)[O-])NCc1cnc(Br)s1
NCC1=CN=C(S1)Br.CNC(SC)=N[N+](=O)[O-].C([O-])([O-])=O.[K+].[K+]>>BrC=1SC(=CN1)CNC(=N[N+](=O)[O-])NC
CS[C:3]([NH:2][CH3:1])=[N:4][N+:5](=[O:6])[O-:7].[NH2:8][CH2:9][c:10]1[cH:11][n:12][c:13]([Br:14])[s:15]1>>[CH3:1][NH:2][C:3](=[N:4][N+:5](=[O:6])[O-:7])[NH:8][CH2:9][c:10]1[cH:11][n:12][c:13]([Br:14])[s:15]1
CNC(=N[N+](=O)[O-])SC.NCc1cnc(Br)s1
CNC(=N[N+](=O)[O-])NCc1cnc(Br)s1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
883fee3f84362c063113a06e86cdc3a3bf94029e9de373b9cf505859a3b7d61a
07cba6ae0650a80cbffb2d3f121f3eee9c0a2be72294ae9df786d5ac7452446b
c1cscn1
C-S-[C;H0;D3;+0:1](-[#7:2]-[C;D1;H3:3])=[#7:4]-[#7;+:5](-[O;-;D1;H0:6])=[O;D1;H0:7].[#16;a:8]:[c:9](-[C:10]-[NH2;D1;+0:11]):[c:12]:[#7;a:13]>>[#16;a:8]:[c:9](-[C:10]-[NH;D2;+0:11]-[C;H0;D3;+0:1](-[#7:2]-[C;D1;H3:3])=[#7:4]-[#7;+:5](-[O;-;D1;H0:6])=[O;D1;H0:7]):[c:12]:[#7;a:13]
null
[]
60
CELSIUS
45
MINUTE
A mixture of 0.39 g of 5-(aminomethyl)-2-bromothiazole, 0.30 g of 1,2-dimethyl-3-nitroisothiourea, 0.58 g of cuprous bromide, 0.55 g of anhydrous potassium carbonate and 4 ml of dry acetonitrile was stirred in an oil bath of 60° C. for 45 minutes. The reaction mixture was purified by a column chromatography [developing...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Primary amine.Monosulfide
Hydrazone.Secondary amine
null
null
c1cscn1
Other
C(C)#N
60
0.75
CNC(=N[N+](=O)[O-])SC.NCc1cnc(Br)s1>C(C)#N>CNC(=N[N+](=O)[O-])NCc1cnc(Br)s1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-3a44a0a0754f42bd896f8b2d41e440db
CSC(=N[N+](=O)[O-])NC(C)=O.NCc1ccc(Cl)nc1>>CC(=O)NC(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
C(C)(=O)NC(SC)=N[N+](=O)[O-].NCC=1C=CC(=NC1)Cl>>C(C)(=O)NC(=N[N+](=O)[O-])NCC=1C=NC(=CC1)Cl
CS[C:5]([NH:4][C:2]([CH3:1])=[O:3])=[N:6][N+:7](=[O:8])[O-:9].[NH2:10][CH2:11][c:12]1[cH:13][cH:14][c:15]([Cl:16])[n:17][cH:18]1>>[CH3:1][C:2](=[O:3])[NH:4][C:5](=[N:6][N+:7](=[O:8])[O-:9])[NH:10][CH2:11][c:12]1[cH:13][cH:14][c:15]([Cl:16])[n:17][cH:18]1
CSC(=N[N+](=O)[O-])NC(C)=O.NCc1ccc(Cl)nc1
CC(=O)NC(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
883fee3f84362c063113a06e86cdc3a3bf94029e9de373b9cf505859a3b7d61a
07cba6ae0650a80cbffb2d3f121f3eee9c0a2be72294ae9df786d5ac7452446b
c1ccncc1
C-S-[C;H0;D3;+0:1](-[#7:2]-[C:3](-[C;D1;H3:4])=[O;D1;H0:5])=[#7:6]-[#7;+:7](-[O;-;D1;H0:8])=[O;D1;H0:9].[#7;a:10]:[c:11]:[c:12]-[C:13]-[NH2;D1;+0:14]>>[#7;a:10]:[c:11]:[c:12]-[C:13]-[NH;D2;+0:14]-[C;H0;D3;+0:1](-[#7:2]-[C:3](-[C;D1;H3:4])=[O;D1;H0:5])=[#7:6]-[#7;+:7](-[O;-;D1;H0:8])=[O;D1;H0:9]
77
[{"value": 77.0, "product": "C(C)(=O)NC(=N[N+](=O)[O-])NCC=1C=NC(=CC1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a mixture of 0.5 g of N-acetyl-S-methyl-N'-nitroisothiourea and 5 ml of acetonitrile was dropwise added a solution of 0.44 g of 5-(aminomethyl)-2-chloropyridine in 3 ml of acetonitrile under ice-cooling, followed by stirring for 30 minutes under ice-cooling. The reaction mixture was concentrated and the residue was ...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Primary amine.Monosulfide
Hydrazone.Secondary amine
null
null
c1ccncc1
Other
C(C)#N
null
0.5
CSC(=N[N+](=O)[O-])NC(C)=O.NCc1ccc(Cl)nc1>C(C)#N>CC(=O)NC(=N[N+](=O)[O-])NCc1ccc(Cl)nc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-386686c9206a4c6aa84bffbf027ce9a8
CC1(C)CC2(CC(C)(C)N1)OC1(CCCCCCCCCCC1)N(CC(O)CN1C(=O)C3(CC(C)(C)NC(C)(C)C3)OC13CCCCCCCCCCC3)C2=O>>CC(=O)OC(CN1C(=O)C2(CC(C)(C)N(C(C)=O)C(C)(C)C2)OC12CCCCCCCCCCC2)CN1C(=O)C2(CC(C)(C)N(C(C)=O)C(C)(C)C2)OC12CCCCCCCCCCC2
OC(CN1C2(OC3(CC(NC(C3)(C)C)(C)C)C1=O)CCCCCCCCCCC2)CN2C1(OC3(CC(NC(C3)(C)C)(C)C)C2=O)CCCCCCCCCCC1>>C(C)(=O)OC(CN1C2(OC3(CC(N(C(C3)(C)C)C(C)=O)(C)C)C1=O)CCCCCCCCCCC2)CN2C1(OC3(CC(N(C(C3)(C)C)C(C)=O)(C)C)C2=O)CCCCCCCCCCC1
[CH3:1][C:2]1([CH3:47])[NH:45][C:42]([CH3:43])([CH3:44])[CH2:41][C:40]2([C:38](=[O:39])[N:37]([CH2:36][CH:5]([OH:4])[CH2:6][N:7]3[C:8](=[O:48])[C:10]4([O:3][C:24]35[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]5)[CH2:11][C:16]([CH3:12])([CH3:17])[NH:15][C:19]([CH3:20])([CH3:21]...
CC1(C)CC2(CC(C)(C)N1)OC1(CCCCCCCCCCC1)N(CC(O)CN1C(=O)C3(CC(C)(C)NC(C)(C)C3)OC13CCCCCCCCCCC3)C2=O
CC(=O)OC(CN1C(=O)C2(CC(C)(C)N(C(C)=O)C(C)(C)C2)OC12CCCCCCCCCCC2)CN1C(=O)C2(CC(C)(C)N(C(C)=O)C(C)(C)C2)OC12CCCCCCCCCCC2
null
null
C(C)(=O)OC(C)=O
Functional Group Addition
OtherReaction
bec8d8226d372e9657754e9deda9f6b7d98c6fb8cff60fac5ce6d3f01bda9190
9938faa317b01ea4d0b81f3f0ca2398d55d079d514fe060b980c46b6aa61685e
O=C1N(CCCN2C(=O)C3(CCNCC3)OC23CCCCCCCCCCC3)C2(CCCCCCCCCCC2)OC12CCNCC2
[C:1]-[C:2]-[C;H0;D4;+0:3]1(-[C:4]-[C:5])-[O;H0;D2;+0:6]-[C;H0;D4;+0:7]2(-[C:8]-[C:9](-[C;D1;H3:10])(-[C;D1;H3:11])-[NH;D2;+0:12]-[C;H0;D4;+0:13](-[C;D1;H3:14])(-[CH3;D1;+0:15])-[CH2;D2;+0:16]-2)-[C;H0;D3;+0:17](=[O;H0;D1;+0:18])-[#7:19]-1-[C:20]-[C:21](-[OH;D1;+0:22])-[C:23]-[#7:24]1-[C:25]-[#8:26]-[C:27]2(-[C:28]-[C:...
null
[]
null
null
null
null
39.2 g of 20,20'-(2-hydroxy-1,3-propanediyl)bis[2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosan-21-one] were dissolved in 400 cm3 of acetic anhydride and heated so strongly that about 200 cm3 of liquid distilled off over the course of 6 hours. The batch was then evaporated to dryness in vacuo, the resid...
10.6084/m9.figshare.5104873.v1
null
Ether.Tertiary amide.Secondary alcohol.Secondary amine.Secondary amine
Ester.Ether.Tertiary amide.Tertiary amide.Tertiary amide
C1CCCCCC2(CCCCC1)[NH]CC1(CCNCC1)O2.C1CCCCCC2(CCCCC1)[NH]CC1(CCNCC1)O2
C1CCCCCC2(CCCCC1)[NH]CC1(CC[NH]CC1)O2.C1CCCCCC2(CCCCC1)[NH]CC1(CC[NH]CC1)O2
C1CCCCCC2(CCCCC1)[NH]CC1(CC[NH]CC1)O2.C1CCCCCC2(CCCCC1)[NH]CC1(CC[NH]CC1)O2
Other
C(C)(=O)OC(C)=O
null
null
CC1(C)CC2(CC(C)(C)N1)OC1(CCCCCCCCCCC1)N(CC(O)CN1C(=O)C3(CC(C)(C)NC(C)(C)C3)OC13CCCCCCCCCCC3)C2=O>C(C)(=O)OC(C)=O>CC(=O)OC(CN1C(=O)C2(CC(C)(C)N(C(C)=O)C(C)(C)C2)OC12CCCCCCCCCCC2)CN1C(=O)C2(CC(C)(C)N(C(C)=O)C(C)(C)C2)OC12CCCCCCCCCCC2
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1a15931d453046db9c51382d25968c1b
N#Cc1ccc(C=O)cc1.O=C1CCCCCC1>>N#Cc1ccc(C=C2CCCCCC2=O)cc1
C(#N)C1=CC=C(C=O)C=C1.C1(CCCCCC1)=O>>C(#N)C1=CC=C(C=C1)C=C1C(CCCCC1)=O
O=[CH:7][c:6]1[cH:5][cH:4][c:3]([C:2]#[N:1])[cH:17][cH:16]1.[CH2:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]1=[O:15]>>[N:1]#[C:2][c:3]1[cH:4][cH:5][c:6]([CH:7]=[C:8]2[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]2=[O:15])[cH:16][cH:17]1
N#Cc1ccc(C=O)cc1.O=C1CCCCCC1
N#Cc1ccc(C=C2CCCCCC2=O)cc1
null
null
P(O)(O)(O)=O
C-C Coupling
Aldol condensation
3dec1fb6f9cde4e05db44511122c36b2d8ebf4e85b66c630348d8cca564268f5
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C1CCCCCC1=Cc1ccccc1
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:10]>>[C:5]-[C:6]-[C;H0;D3;+0:7](=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[C:8](=[O;D1;H0:9])-[C:10]
null
[]
100
CELSIUS
null
null
A mixture of 20.0 g of 4-cyanobenzaldehyde, 30.5 g of cycloheptanone, and 200 mL of 85% phosphoric acid is heated for 1.5 h at 100° C. The mixture is cooled to room temperature, and filtered. The filtrate is poured into water (800 mL), and the precipitate is filtered, washed with water, and dried. The solid is purified...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
C1CCCCCC1
C1CCCCCC1
c1ccccc1.C1CCCCCC1
HO-
P(O)(O)(O)=O
100
null
N#Cc1ccc(C=O)cc1.O=C1CCCCCC1>P(O)(O)(O)=O>N#Cc1ccc(C=C2CCCCCC2=O)cc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-2727f5fbd06a4d3584654f6341198823
COc1ccc(Br)cc1C=O.NO>>COc1ccc(Br)cc1C#N
[OH-].[Na+].BrC1=CC=C(C(C=O)=C1)OC.Cl.NO.C(=O)[O-].[Na+]>>BrC=1C=CC(=C(C#N)C1)OC
O=[CH:10][c:9]1[c:3]([O:2][CH3:1])[cH:4][cH:5][c:6]([Br:7])[cH:8]1.O[NH2:11]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([Br:7])[cH:8][c:9]1[C:10]#[N:11]
COc1ccc(Br)cc1C=O.NO
COc1ccc(Br)cc1C#N
null
null
C(=O)O
Miscellaneous
OtherReaction
748a00525e7f639e600a6b1229bb8ce947b6e2e96d815c0b05b54470e6cdbc2a
a27285857ea2428fb666a281ae1a2b961eec077cb33a106e48534c99bfe3d865
c1ccccc1
O-[NH2;D1;+0:1].O=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[N;H0;D1;+0:1]#[C;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
100
CELSIUS
1
HOUR
A mixture of 6.45 g 5-bromo-o-anisaldehyde, 2.2 g of hydroxylamine hydrochloride, 4.1 g of sodium formate and 20 mL formic acid were heated at 100° C. with stirring for 1 h. The reaction mixture was poured onto ice water and the mixture was made basic by the careful addition of 50% sodium hydroxide. The product was ext...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Primary amine
Nitrile
null
null
c1ccccc1
HO-
C(=O)O
100
1
COc1ccc(Br)cc1C=O.NO>C(=O)O>COc1ccc(Br)cc1C#N
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-d114fb2eb83049129c2f8def69a7c116
COc1cccc(C#N)c1OC.C[Si](C)(C)N[Si](C)(C)C>>COc1cccc(C(=N)N)c1OC
Cl.C[Si](N[Si](C)(C)C)(C)C.C(CCC)[Li].COC1=C(C#N)C=CC=C1OC>>COC1=C(C(=N)N)C=CC=C1OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8]#[N:9])[c:11]1[O:12][CH3:13].C[Si](C)(C)[NH:10][Si](C)(C)C>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[NH:9])[NH2:10])[c:11]1[O:12][CH3:13]
COc1cccc(C#N)c1OC.C[Si](C)(C)N[Si](C)(C)C
COc1cccc(C(=N)N)c1OC
null
null
CCCCCC.CCOCC
Heteroatom Alkylation and Arylation
OtherReaction
c69dc3918ec11d93fc440abf3e0b6efc258614217c8cf5c36cff1eaf4ee3899f
827d5e8a7cbda8ac46afd217e51ef2b5ed64b3899fb0f9044671ad16df2d1214
c1ccccc1
C-[Si](-C)(-C)-[NH;D2;+0:1]-[Si](-C)(-C)-C.[N;H0;D1;+0:2]#[C;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]>>[NH2;D1;+0:1]-[C;H0;D3;+0:3](=[NH;D1;+0:2])-[c:4](:[c:5]):[c:6]
null
[]
null
null
10
MINUTE
To a solution of 20 g 1,1,1,3,3,3-hexamethyldisilazane in 150 mL dry ether was added 5 mL 2.4M n-butyllithium in hexane. After 10 min at room temperature, 16.3 g 2,3-dimethoxybenzonitrile was added in one portion and the mixture was kept at room temperature for 16 h. The reaction mixture was then poured onto excess 3N ...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Secondary amine.Silyl protective group.Silyl protective group
Primary amine
null
null
c1ccccc1
Other
CCCCCC.CCOCC
null
0.166667
COc1cccc(C#N)c1OC.C[Si](C)(C)N[Si](C)(C)C>CCCCCC.CCOCC>COc1cccc(C(=N)N)c1OC
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-0625e72398ed4dd58710646ee2d5a082
COS(=O)(=O)OC.c1ccc(-c2ncc[nH]2)cc1>>Cn1ccnc1-c1ccccc1
[Cl-].[NH4+].C1(=CC=CC=C1)C=1NC=CN1.C(C)(C)[N-]C(C)C.[Li+].S(=O)(=O)(OC)OC>>CN1C(=NC=C1)C1=CC=CC=C1
COS(=O)(=O)O[CH3:1].[nH:2]1[cH:3][cH:4][n:5][c:6]1-[c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1>>[CH3:1][n:2]1[cH:3][cH:4][n:5][c:6]1-[c:7]1[cH:8][cH:9][cH:10][cH:11][cH:12]1
COS(=O)(=O)OC.c1ccc(-c2ncc[nH]2)cc1
Cn1ccnc1-c1ccccc1
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
N-methylation
cd2ba7d8131691ffcb15dc3ca1da5447edd8b78d140f3b82779a267b9d6114c9
7a358c636daddc97c1fb4c29f378044d7eac3f01815d9966e599841f642d631a
c1ccc(-c2ncc[nH]2)cc1
C-O-S(=O)(=O)-O-[CH3;D1;+0:1].[c:2]-[c:3]1:[#7;a:4]:[c:5]:[c:6]:[nH;D2;+0:7]:1>>[CH3;D1;+0:1]-[n;H0;D3;+0:7]1:[c:6]:[c:5]:[#7;a:4]:[c:3]:1-[c:2]
null
[]
0
CELSIUS
10
MINUTE
A solution of 40 mL tetrahydrofuran containing 1.0 g of 2-phenylimidazole was cooled to 0° C. and 4 mL of 2M lithium diisopropylamide was added dropwise which resulted in the formation of a white suspension. The mixture was stirred for 10 min at 0° C. and then 0.7 mL of dimethyl sulfate was added. The reaction was allo...
10.6084/m9.figshare.5104873.v1
null
null
null
c1c[nH]cn1
c1ncc[nH]1
c1ncc[nH]1.c1ccccc1
HO-
O1CCCC1
0
0.166667
COS(=O)(=O)OC.c1ccc(-c2ncc[nH]2)cc1>O1CCCC1>Cn1ccnc1-c1ccccc1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-2c0cc496a601484484a0b9ec05dbbaef
C=O.Cc1c[nH]c(-c2ccccc2)n1.c1ccc(CC2CCNCC2)cc1>>Cc1[nH]c(-c2ccccc2)nc1CN1CCC(Cc2ccccc2)CC1
CC=1N=C(NC1)C1=CC=CC=C1.C=O.C(C1=CC=CC=C1)C1CCNCC1>>CC1=C(N=C(N1)C1=CC=CC=C1)CN1CCC(CC1)CC1=CC=CC=C1
O=[CH2:13].[CH3:1][c:2]1[n:3][c:4](-[c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[nH:11][cH:12]1.[NH:14]1[CH2:15][CH2:16][CH:17]([CH2:18][c:19]2[cH:20][cH:21][cH:22][cH:23][cH:24]2)[CH2:25][CH2:26]1>>[CH3:1][c:2]1[nH:3][c:4](-[c:5]2[cH:6][cH:7][cH:8][cH:9][cH:10]2)[n:11][c:12]1[CH2:13][N:14]1[CH2:15][CH2:16][CH:17]([CH2:18][...
C=O.Cc1c[nH]c(-c2ccccc2)n1.c1ccc(CC2CCNCC2)cc1
Cc1[nH]c(-c2ccccc2)nc1CN1CCC(Cc2ccccc2)CC1
null
null
C(C)(=O)O
Heteroatom Alkylation and Arylation
OtherReaction
96776234213b3dd2b36e241fe4b7b05149b775b962c3ecc7a824743adfb94abd
e1fdef8fde1c506d7c9deb8fd5e6f322eceea2abce3167abcf412a1fa4fd5443
c1ccc(CC2CCN(Cc3c[nH]c(-c4ccccc4)n3)CC2)cc1
O=[CH2;D1;+0:1].[C;D1;H3:2]-[c:3]1:[cH;D2;+0:4]:[nH;D2;+0:5]:[c:6](-[c:7]):[n;H0;D2;+0:8]:1.[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]>>[C:9]-[C:10]-[N;H0;D3;+0:11](-[CH2;D2;+0:1]-[c;H0;D3;+0:4]1:[n;H0;D2;+0:5]:[c:6](-[c:7]):[nH;D2;+0:8]:[c:3]:1-[C;D1;H3:2])-[C:12]-[C:13]
null
[]
100
CELSIUS
null
null
To a solution of 1 g of 1 methyl-2-phenylimidazole in 10 mL acetic acid were added 0.4 mL of 37% aqueous formaldehyde and 1.2 mL of 4-benzylpiperidine. The reaction mixture was heated at 100° C. for 10 hours and the acetic acid then removed by evaporated under reduced pressure. The residue was dissolved in water and ma...
10.6084/m9.figshare.5104873.v1
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Formaldehyde.Secondary amine
Tertiary amine
c1c[nH]cn1.C1CCNCC1
c1c[nH]cn1.C1CC[NH]CC1
c1c[nH]cn1.c1ccccc1.C1CC[NH]CC1.c1ccccc1
HO-
C(C)(=O)O
100
null
C=O.Cc1c[nH]c(-c2ccccc2)n1.c1ccc(CC2CCNCC2)cc1>C(C)(=O)O>Cc1[nH]c(-c2ccccc2)nc1CN1CCC(Cc2ccccc2)CC1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-21a6de5b6dff4930a1b4971decc73307
CC(=O)[O-].CCNC(=O)C([O-])=S.NCC(=O)c1ccccc1>>CCOC(=O)c1nc(-c2ccccc2)c[nH]1
C(C)(=O)O.C(C)NC(C(=S)[O-])=O.Cl.NCC(=O)C1=CC=CC=C1.C(C)(=O)[O-].[Na+]>>C1(=CC=CC=C1)C=1N=C(NC1)C(=O)OCC
CC(=O)[O-:3].O=[C:6]([C:4](=S)[O-:5])[NH:7][CH2:2][CH3:1].O=[C:8]([c:9]1[cH:10][cH:11][cH:12][cH:13][cH:14]1)[CH2:15][NH2:16]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[c:6]1[n:7][c:8](-[c:9]2[cH:10][cH:11][cH:12][cH:13][cH:14]2)[cH:15][nH:16]1
CC(=O)[O-].CCNC(=O)C([O-])=S.NCC(=O)c1ccccc1
CCOC(=O)c1nc(-c2ccccc2)c[nH]1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
5a82c0f043645883ee69c1e8cf46e171d7ccd1fb94c2b266e1cb042f87a3c180
bd2e4ae1a43ea793c5148ee7f3f6f0b005b5e2df6bfa3d3ebe2f20fff7f21e30
c1ccc(-c2c[nH]cn2)cc1
C-C(=O)-[O-;H0;D1:1].O=[C;H0;D3;+0:2](-[CH2;D2;+0:3]-[NH2;D1;+0:4])-[c;H0;D3;+0:5](:[c:6]:[c:7]):[c:8]:[c:9].O=[C;H0;D3;+0:10](-[NH;D2;+0:11]-[CH2;D2;+0:12]-[C;D1;H3:13])-[C;H0;D3;+0:14](=S)-[O-;H0;D1:15]>>[C;D1;H3:13]-[CH2;D2;+0:12]-[O;H0;D2;+0:1]-[C;H0;D3;+0:14](=[O;H0;D1;+0:15])-[c;H0;D3;+0:10]1:[n;H0;D2;+0:11]:[c;H...
null
[]
null
null
null
null
A mixture of 3 g of ethylthiooxamate, 4.25 g of 2-aminoacetophenone hydrochloride and 3.69 g of sodium acetate was dissolved in 20 mL of acetic acid and heated under reflux for 3 hr. The reaction mixture was allowed to cool to room temperature and the acetic acid removed by evaporation under reduced pressure. The resid...
10.6084/m9.figshare.5104873.v1
null
Ketone.Secondary amide.Primary amine.Thiocarbonyl
Ester
null
c1c[nH]cn1
c1c[nH]cn1.c1ccccc1
Other
null
null
null
CC(=O)[O-].CCNC(=O)C([O-])=S.NCC(=O)c1ccccc1>>CCOC(=O)c1nc(-c2ccccc2)c[nH]1
ord_dataset-c2ad1656a3ca4d08888ffb6e3f3a2742
ord-1e5b9dea2807444dbd3f6f54b251d447
CCOC(=O)c1nc(-c2ccccc2)c[nH]1>>OCc1nc(-c2ccccc2)c[nH]1
C(C)OC(=O)C=1NC=C(N1)C1=CC=CC=C1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>>OCC=1NC=C(N1)C1=CC=CC=C1
CCO[C:2](=[O:1])[c:3]1[n:4][c:5](-[c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[cH:12][nH:13]1>>[OH:1][CH2:2][c:3]1[n:4][c:5](-[c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[cH:12][nH:13]1
CCOC(=O)c1nc(-c2ccccc2)c[nH]1
OCc1nc(-c2ccccc2)c[nH]1
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc(-c2c[nH]cn2)cc1
C-C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3]1:[#7;a:4]:[c:5]:[c:6]:[#7;a:7]:1>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3]1:[#7;a:4]:[c:5]:[c:6]:[#7;a:7]:1
90.3
[{"value": 90.3, "product": "OCC=1NC=C(N1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of 2.75 g ethyl-4-phenylimidazole-2-carboxylate in 20 mL tetrahydrofuran was added a suspension of 0.5 g lithium aluminum hydride in 30 mL of tetrahydrofuran. The reaction mixture was stirred at room temperature overnight, poured into 100 mL of ice water and extracted with 2 x I00 mL of ethyl acetate. The...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1c[nH]cn1.c1ccccc1
HO-
O1CCCC1
null
8
CCOC(=O)c1nc(-c2ccccc2)c[nH]1>O1CCCC1>OCc1nc(-c2ccccc2)c[nH]1