dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-15d9dcd887d94a9aa3a4e3d1faabafd1
Clc1ncnc2cc[nH]c12.O=C(OCC(CBr)OC(=O)c1ccccc1)c1ccccc1>>O=C(OCC(Cn1ccc2ncnc(Cl)c21)OC(=O)c1ccccc1)c1ccccc1
ClC=1C2=C(N=CN1)C=CN2.C(C1=CC=CC=C1)(=O)OCC(CBr)OC(C1=CC=CC=C1)=O.C([O-])([O-])=O.[Cs+].[Cs+].CN(C=O)C>>C(C1=CC=CC=C1)(=O)OCC(CN1C=CC=2N=CN=C(C21)Cl)OC(C2=CC=CC=C2)=O
[nH:7]1[cH:8][cH:9][c:10]2[n:11][cH:12][n:13][c:14]([Cl:15])[c:16]12.Br[CH2:6][CH:5]([CH2:4][O:3][C:2](=[O:1])[c:26]1[cH:27][cH:28][cH:29][cH:30][cH:31]1)[O:17][C:18](=[O:19])[c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[O:1]=[C:2]([O:3][CH2:4][CH:5]([CH2:6][n:7]1[cH:8][cH:9][c:10]2[n:11][cH:12][n:13][c:14]([Cl:15])[c:...
Clc1ncnc2cc[nH]c12.O=C(OCC(CBr)OC(=O)c1ccccc1)c1ccccc1
O=C(OCC(Cn1ccc2ncnc(Cl)c21)OC(=O)c1ccccc1)c1ccccc1
null
null
C(C)(=O)OCC
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
ecfdd3ebe7f504d096c44af08936ff56b52d45d78f82ef9c3a3c3047f20010b5
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=C(OCC(Cn1ccc2ncncc21)OC(=O)c1ccccc1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](-[C:3])-[#8:4]-[C:5]=[O;D1;H0:6].[Cl;D1;H0:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]2:[c:13]:[c:14]:[nH;D2;+0:15]:[c:16]:2:1>>[C:3]-[C:2](-[#8:4]-[C:5]=[O;D1;H0:6])-[CH2;D2;+0:1]-[n;H0;D3;+0:15]1:[c:14]:[c:13]:[c:12]2:[#7;a:11]:[c:10]:[#7;a:9]:[c:8](-[Cl;D1;H0:7]):[c:16]:2:1
28.3
[{"value": 28.3, "product": "C(C1=CC=CC=C1)(=O)OCC(CN1C=CC=2N=CN=C(C21)Cl)OC(C2=CC=CC=C2)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
4
HOUR
A mixture of 4-chloro-5H-pyrrolo[3,2-d]pyrimidine (500 mg), 3-bromopropane-1,2-diyl dibenzoate (1.77 g), cesium carbonate (1.59 g) and N,N-dimethylformamide (6.5 mL) was stirred at 80° C. for 4 hrs. The reaction mixture was diluted with ethyl acetate (100 mL) and washed with water (80 mL). The organic layer was separat...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1ncc2[nH]ccc2n1
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HBr
C(C)(=O)OCC
80
4
Clc1ncnc2cc[nH]c12.O=C(OCC(CBr)OC(=O)c1ccccc1)c1ccccc1>C(C)(=O)OCC>O=C(OCC(Cn1ccc2ncnc(Cl)c21)OC(=O)c1ccccc1)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-7a8c24dac5c44e08bce93d42fbb68e1b
CN(C(=O)C(F)(F)F)c1c(I)ncnc1I.N#Cc1cccc(Oc2ccc(N)cc2Cl)c1>>CN(C(=O)C(F)(F)F)c1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
IC1=NC=NC(=C1N(C(C(F)(F)F)=O)C)I.NC1=CC(=C(OC=2C=C(C#N)C=CC2)C=C1)Cl.C(O)([O-])=O.[Na+]>>ClC=1C=C(C=CC1OC1=CC(=CC=C1)C#N)NC1=NC=NC(=C1N(C(C(F)(F)F)=O)C)I
I[c:15]1[c:9]([N:2]([CH3:1])[C:3](=[O:4])[C:5]([F:6])([F:7])[F:8])[c:10]([I:11])[n:12][cH:13][n:14]1.[NH2:16][c:17]1[cH:18][cH:19][c:20]([O:21][c:22]2[cH:23][cH:24][cH:25][c:26]([C:27]#[N:28])[cH:29]2)[c:30]([Cl:31])[cH:32]1>>[CH3:1][N:2]([C:3](=[O:4])[C:5]([F:6])([F:7])[F:8])[c:9]1[c:10]([I:11])[n:12][cH:13][n:14][c:1...
CN(C(=O)C(F)(F)F)c1c(I)ncnc1I.N#Cc1cccc(Oc2ccc(N)cc2Cl)c1
CN(C(=O)C(F)(F)F)c1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
null
null
CN1C(CCC1)=O
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c38b7155556ff28144ae37859ff6668b20d59da60c705d26b158542b6d8385da
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(Oc2ccc(Nc3ccncn3)cc2)cc1
I-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5](-[I;D1;H0:6]):[c:7]:1-[#7:8]-[C:9]=[O;D1;H0:10].[NH2;D1;+0:11]-[c:12](:[c:13]):[c:14]>>[I;D1;H0:6]-[c:5]1:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:11]-[c:12](:[c:13]):[c:14]):[c:7]:1-[#7:8]-[C:9]=[O;D1;H0:10]
44.3
[{"value": 44.3, "product": "ClC=1C=C(C=CC1OC1=CC(=CC=C1)C#N)NC1=NC=NC(=C1N(C(C(F)(F)F)=O)C)I", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
100
CELSIUS
null
null
N-(4,6-Diiodopyrimidin-5-yl)-2,2,2-trifluoro-N-methylacetamide (3 g) and 3-(4-amino-2-chlorophenoxy)benzonitrile (1.69 g) were dissolved in 1-methyl-2-pyrrolidone (11.4 mL), and the mixture was stirred with heating at 100° C. for 16 hrs. To the reaction mixture was added aqueous sodium hydrogen carbonate (80 mL) and th...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1cncnc1
c1cncnc1
c1cncnc1.c1ccccc1.c1ccccc1
HI
CN1C(CCC1)=O
100
null
CN(C(=O)C(F)(F)F)c1c(I)ncnc1I.N#Cc1cccc(Oc2ccc(N)cc2Cl)c1>CN1C(CCC1)=O>CN(C(=O)C(F)(F)F)c1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ecf93b431f3f4e69b4a56b01fcadb82b
CN(C(=O)C(F)(F)F)c1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1>>CNc1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
C(C)(=O)OCC.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C#N)NC1=NC=NC(=C1N(C(C(F)(F)F)=O)C)I.[BH4-].[Na+]>>ClC1=C(OC=2C=C(C#N)C=CC2)C=CC(=C1)NC1=NC=NC(=C1NC)I
O=C(C(F)(F)F)[N:2]([CH3:1])[c:3]1[c:4]([I:5])[n:6][cH:7][n:8][c:9]1[NH:10][c:11]1[cH:12][cH:13][c:14]([O:15][c:16]2[cH:17][cH:18][cH:19][c:20]([C:21]#[N:22])[cH:23]2)[c:24]([Cl:25])[cH:26]1>>[CH3:1][NH:2][c:3]1[c:4]([I:5])[n:6][cH:7][n:8][c:9]1[NH:10][c:11]1[cH:12][cH:13][c:14]([O:15][c:16]2[cH:17][cH:18][cH:19][c:20](...
CN(C(=O)C(F)(F)F)c1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
CNc1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
null
null
C(C)(C)O.O1CCCC1
Reduction
Hydrogenolysis of tertiary amines
16961a3d99942c0ab361f2149cf4766848c112f4d4d9e5e515a20194fa44ecb0
9d0759623d33e2d41aafe1af3bb1025d4d7a88f20060c872279b889c110cab65
c1ccc(Oc2ccc(Nc3ccncn3)cc2)cc1
F-C(-F)(-F)-C(=O)-[N;H0;D3;+0:1](-[C;D1;H3:2])-[c:3]1:[c:4](-[I;D1;H0:5]):[#7;a:6]:[c:7]:[#7;a:8]:[c:9]:1-[#7:10]>>[#7:10]-[c:9]1:[#7;a:8]:[c:7]:[#7;a:6]:[c:4](-[I;D1;H0:5]):[c:3]:1-[NH;D2;+0:1]-[C;D1;H3:2]
90.7
[{"value": 90.7, "product": "ClC1=C(OC=2C=C(C#N)C=CC2)C=CC(=C1)NC1=NC=NC(=C1NC)I", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
To a solution of N-(4-{[3-chloro-4-(3-cyanophenoxy)phenyl]amino}-6-iodopyrimidin-5-yl)-2,2,2-trifluoro-N-methylacetamide (1.0 g) in isopropanol-tetrahydrofuran (5.0 mL-10 mL) was added sodium borohydride (70 mg) at room temperature. The mixture was stirred at room temperature for 1.5 hrs, and ethyl acetate was added. T...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Tertiary amide
Secondary amine
null
null
c1cncnc1.c1ccccc1.c1ccccc1
Other
C(C)(C)O.O1CCCC1
null
1.5
CN(C(=O)C(F)(F)F)c1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1>C(C)(C)O.O1CCCC1>CNc1c(I)ncnc1Nc1ccc(Oc2cccc(C#N)c2)c(Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-72c172c741374100bf28532885c01fb5
COS(C)(=O)=O.Nc1c(I)ncnc1I>>CNc1c(I)ncnc1I
C(C)(=O)OCC.CS(=O)(=O)OC.IC1=NC=NC(=C1N)I.[H-].[Na+]>>IC1=NC=NC(=C1NC)I
CS(=O)(=O)O[CH3:1].[NH2:2][c:3]1[c:4]([I:5])[n:6][cH:7][n:8][c:9]1[I:10]>>[CH3:1][NH:2][c:3]1[c:4]([I:5])[n:6][cH:7][n:8][c:9]1[I:10]
COS(C)(=O)=O.Nc1c(I)ncnc1I
CNc1c(I)ncnc1I
null
null
O1CCCC1
Heteroatom Alkylation and Arylation
Alkylation of amines
8445343b2fb2fd8a9bc06f8532794f2ba6b99565a6e05a3bb9a4344ce2671186
7e6303acde8be57b43b4c6a673e1c7537b1efde90f08932e09e153dbba53a700
c1cncnc1
C-S(=O)(=O)-O-[CH3;D1;+0:1].[I;D1;H0:2]-[c:3]1:[#7;a:4]:[c:5]:[#7;a:6]:[c:7](-[I;D1;H0:8]):[c:9]:1-[NH2;D1;+0:10]>>[CH3;D1;+0:1]-[NH;D2;+0:10]-[c:9]1:[c:7](-[I;D1;H0:8]):[#7;a:6]:[c:5]:[#7;a:4]:[c:3]:1-[I;D1;H0:2]
null
[]
null
null
30
MINUTE
To a solution of 4,6-diiodopyrimidin-5-amine (1.0 g) in tetrahydrofuran (10 mL) was added sodium hydride (60%, 138 mg) under ice-cooling. The mixture was stirred at room temperature for 30 min. To the reaction system was added dropwise a solution of methyl methanesulfonate (0.256 mL) in tetrahydrofuran (4.0 mL). The mi...
10.6084/m9.figshare.5104873.v1
null
Mesylate.Primary amine
Secondary amine
null
null
c1cncnc1
MsOH.HO-
O1CCCC1
null
0.5
COS(C)(=O)=O.Nc1c(I)ncnc1I>O1CCCC1>CNc1c(I)ncnc1I
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-79d8f9174b804d84b1fa5b73fbf2f019
CC(C)(CO)C(=O)O.NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>CC(C)(CO)C(=O)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl.OCC(C(=O)O)(C)C.Cl.C(C)N=C=NCCCN(C)C.O.ON1N=NC2=C1C=CC=C2>>Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(C(CO)(C)C)=O
O[C:6]([C:2]([CH3:1])([CH3:3])[CH2:4][OH:5])=[O:7].[NH2:8][CH2:9][CH2:10][n:11]1[cH:12][cH:13][c:14]2[n:15][cH:16][n:17][c:18]([NH:19][c:20]3[cH:21][cH:22][c:23]([O:24][c:25]4[cH:26][cH:27][cH:28][c:29]([C:30]([F:31])([F:32])[F:33])[cH:34]4)[c:35]([Cl:36])[cH:37]3)[c:38]12>>[CH3:1][C:2]([CH3:3])([CH2:4][OH:5])[C:6](=[O...
CC(C)(CO)C(=O)O.NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
CC(C)(CO)C(=O)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
O.C(C)N(CC)CC.CN(C=O)C
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C;D1;H3:5])-[C;D1;H3:6].[C:7]-[C:8]-[NH2;D1;+0:9]>>[C:7]-[C:8]-[NH;D2;+0:9]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C:4])(-[C;D1;H3:5])-[C;D1;H3:6]
141.4
[{"value": 141.4, "product": "Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(C(CO)(C)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
HOUR
A solution of 5-(2-aminoethyl)-N-{3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride (150 mg), 3-hydroxy-2,2-dimethylpropanoic acid (68 mg), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (166 mg), 1-hydroxybenzotriazole monohydrate (132 mg) and triethylamine ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HO-
O.C(C)N(CC)CC.CN(C=O)C
null
15
CC(C)(CO)C(=O)O.NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>O.C(C)N(CC)CC.CN(C=O)C>CC(C)(CO)C(=O)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-65461c604e27486ea7313b751fc8862c
Cc1ccc(S(=O)(=O)O)cc1>>Cc1ccc(S(=O)(=O)O)cc1
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CS(=O)(=O)C)=O.O.CC1=CC=C(C=C1)S(=O)(=O)O>>CC1=CC=C(C=C1)S(=O)(=O)O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CS(=O)(=O)C)=O
[CH3:39][c:40]1[cH:41][cH:42][c:43]([S:44](=[O:45])(=[O:46])[OH:47])[cH:48][cH:49]1>>[CH3:39][c:40]1[cH:41][cH:42][c:43]([S:44](=[O:45])(=[O:46])[OH:47])[cH:48][cH:49]1
Cc1ccc(S(=O)(=O)O)cc1
Cc1ccc(S(=O)(=O)O)cc1
null
null
C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccccc1
null
76.9
[{"value": 76.9, "product": "CC1=CC=C(C=C1)S(=O)(=O)O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CS(=O)(=O)C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
To a solution of N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-2-(methylsulfonyl)acetamide (150 mg) in ethyl acetate (10 mL) was added 4-methylbenzenesulfonic acid monohydrate (55.4 mg) at room temperature. The mixture was stirred at room temperature for 20 hrs, a...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1
null
C(C)(=O)OCC
null
20
Cc1ccc(S(=O)(=O)O)cc1>C(C)(=O)OCC>Cc1ccc(S(=O)(=O)O)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-dbc2033accfe4a1fb1f00e519e28f15c
CC(Cn1ccc2ncnc(Cl)c21)NC(=O)OC(C)(C)C.Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1>>CC(N)Cn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21.Cl
C(=O)(OC(C)(C)C)OC(=O)OC(C)(C)C.C(C)(C)(C)OC(NC(CN1C=CC=2N=CN=C(C21)Cl)C)=O.ClC=1C=C(N)C=CC1OC1=CC(=CC=C1)C(F)(F)F.Cl>>Cl.Cl.NC(CN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl)C
CC(C)(C)OC(=O)[NH:3][CH:2]([CH3:1])[CH2:4][n:5]1[cH:6][cH:7][c:8]2[n:9][cH:10][n:11][c:12]([Cl:34])[c:32]12.[NH2:13][c:14]1[cH:15][cH:16][c:17]([O:18][c:19]2[cH:20][cH:21][cH:22][c:23]([C:24]([F:25])([F:26])[F:27])[cH:28]2)[c:29]([Cl:30])[cH:31]1>>[CH3:1][CH:2]([NH2:3])[CH2:4][n:5]1[cH:6][cH:7][c:8]2[n:9][cH:10][n:11][...
CC(Cn1ccc2ncnc(Cl)c21)NC(=O)OC(C)(C)C.Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1
CC(N)Cn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21.Cl
null
null
O1CCCC1.O.C(C)N(CC)CC.CN1C(CCC1)=O
Heteroatom Alkylation and Arylation
OtherReaction
52eabfea8525971db681e2ff459bf7eb578389257f19a2ae4aa6823100bd47a3
b189e21881719932ff7e93d2cee73d5d9b679e27f974877dd5fa270130c3c7ff
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C;D1;H3:3])-[C:4]-[#7;a:5]1:[c:6]:[c:7]:[c:8]2:[#7;a:9]:[c:10]:[#7;a:11]:[c;H0;D3;+0:12](-[Cl;H0;D1;+0:13]):[c:14]:1:2.[NH2;D1;+0:15]-[c:16](:[c:17]):[c:18]>>[C;D1;H3:3]-[C:2](-[NH2;D1;+0:1])-[C:4]-[#7;a:5]1:[c:6]:[c:7]:[c:8]2:[#7;a:9]:[c:10]:[#7;a:11]:[c;H0;D3;+0:12](-[NH;D2;+0...
57.2
[{"value": 57.2, "product": "Cl.Cl.NC(CN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
20
HOUR
A solution of tert-butyl[2-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-5-yl)-1-methylethyl]carbamate (350 mg) and 3-chloro-4-[3-(trifluoromethyl)phenoxy]aniline (423 mg) in 1-methyl-2-pyrrolidone (3.5 mL) was stirred at 120° C. for 4 hrs. After cooling to room temperature, triethylamine (0.24 mL) and di-tert-butyl dicarbonate...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Primary amine.Boc
Primary amine.Secondary amine
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HO-
O1CCCC1.O.C(C)N(CC)CC.CN1C(CCC1)=O
null
20
CC(Cn1ccc2ncnc(Cl)c21)NC(=O)OC(C)(C)C.Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1>O1CCCC1.O.C(C)N(CC)CC.CN1C(CCC1)=O>CC(N)Cn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c6b55629e401480eb9c9dd6f626fafe0
CS(=O)(=O)O>>CS(=O)(=O)O
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CC(C)(C)O)=O.CS(=O)(=O)O>>CS(=O)(=O)O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CC(C)(C)O)=O
[CH3:39][S:40](=[O:41])(=[O:42])[OH:43]>>[CH3:39][S:40](=[O:41])(=[O:42])[OH:43]
CS(=O)(=O)O
CS(=O)(=O)O
null
null
C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
null
null
null
[]
null
null
1
HOUR
To a solution of N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxy-3-methylbutanamide (200 mg) in ethyl acetate (10 mL) was added methanesulfonic acid (26 μL) at room temperature. The mixture was stirred at room temperature for 1 hr and concentrated under re...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
null
null
C(C)(=O)OCC
null
1
CS(=O)(=O)O>C(C)(=O)OCC>CS(=O)(=O)O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-895c14f759f5434c80c0ce33d78542f9
O=C1c2ccccc2C(=O)N1CCOCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>CC(=O)NCCOCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCOCCN2C(C1=CC=CC=C1C2=O)=O.O.NN.C(O)([O-])=O.[Na+]>>ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCOCCNC(C)=O
O=C1c2cccc[c:1]2[C:2](=[O:3])[N:4]1[CH2:5][CH2:6][O:7][CH2:8][CH2:9][n:10]1[cH:11][cH:12][c:13]2[n:14][cH:15][n:16][c:17]([NH:18][c:19]3[cH:20][cH:21][c:22]([O:23][c:24]4[cH:25][cH:26][cH:27][c:28]([C:29]([F:30])([F:31])[F:32])[cH:33]4)[c:34]([Cl:35])[cH:36]3)[c:37]12>>[CH3:1][C:2](=[O:3])[NH:4][CH2:5][CH2:6][O:7][CH2:...
O=C1c2ccccc2C(=O)N1CCOCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
CC(=O)NCCOCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
C(C)O
Reduction
OtherReaction
d9171dbb22691e73cd44616f21fa6dcc09b4c3cd8ebc10a38d0adf93000789a7
15328f7911cf420e5b98cd32bf65857f1b0cf0d0f9e28f1ac7b23b1642c85385
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
O=C1-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4](=[O;D1;H0:5])-[c;H0;D3;+0:6]2:c:c:c:c:c:2-1>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4](-[CH3;D1;+0:6])=[O;D1;H0:5]
85
[{"value": 85.0, "product": "ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCOCCNC(C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
2-(2-{2-[4-({3-Chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethoxy}ethyl)-1H-isoindole-1,3(2H)-dione (200 mg) was dissolved in ethanol (5.0 mL), hydrazine monohydrate (3.0 mL) was added, and the mixture was stirred for 1 hr. To the reaction mixture was added saturated aqueous sodiu...
10.6084/m9.figshare.5104873.v1
null
Substituted dicarboximide
Secondary amide
c1ccc2c(c1)C[NH]C2
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
Other
C(C)O
null
1
O=C1c2ccccc2C(=O)N1CCOCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>C(C)O>CC(=O)NCCOCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d02c53dd9aa349dfa54725c51b49d7d6
C=CC(=O)OCC.Clc1ncnc2cc[nH]c12>>CCOC(=O)CCn1ccc2ncnc(Cl)c21
C(C=C)(=O)OCC.[Cl-].[NH4+].C(C=C)(=O)OCC.C([O-])([O-])=O.[K+].[K+].C(C=C)(=O)OCC.C([O-])([O-])=O.[K+].[K+].ClC=1C2=C(N=CN1)C=CN2>>ClC=1C2=C(N=CN1)C=CN2CCC(=O)OCC
[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]=[CH2:7].[nH:8]1[cH:9][cH:10][c:11]2[n:12][cH:13][n:14][c:15]([Cl:16])[c:17]12>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][CH2:7][n:8]1[cH:9][cH:10][c:11]2[n:12][cH:13][n:14][c:15]([Cl:16])[c:17]12
C=CC(=O)OCC.Clc1ncnc2cc[nH]c12
CCOC(=O)CCn1ccc2ncnc(Cl)c21
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
OtherReaction
4630ca5b1c48d0db9b828625c844c1c8a6e34988bffd712ddc4b008089593e34
51fad62e29f5f77e8a2cefce7ceeba2655475fda67fa72d63935019e1a813761
c1ncc2[nH]ccc2n1
[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH;D2;+0:5]=[CH2;D1;+0:6].[Cl;D1;H0:7]-[c:8]1:[#7;a:9]:[c:10]:[#7;a:11]:[c:12]2:[c:13]:[c:14]:[nH;D2;+0:15]:[c:16]:2:1>>[C:1]-[#8:2]-[C:3](=[O;D1;H0:4])-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[n;H0;D3;+0:15]1:[c:14]:[c:13]:[c:12]2:[#7;a:11]:[c:10]:[#7;a:9]:[c:8](-[Cl;D1;H0:7]):[c:16]:2:1
null
[]
null
null
7.5
HOUR
4-Chloro-5H-pyrrolo[3,2-d]pyrimidine (303 mg) was dissolved in N,N-dimethylformamide (9 mL), ethyl acrylate (0.3 mL) and potassium carbonate (538 mg) were sequentially added, and the mixture was stirred at room temperature for 7.5 hrs. Ethyl acrylate (0.2 mL) was added, and the mixture was stirred for 16 hrs. Ethyl acr...
10.6084/m9.figshare.5104873.v1
null
Ester.Vinyl
Ester
c1ncc2[nH]ccc2n1
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
null
CN(C=O)C
null
7.5
C=CC(=O)OCC.Clc1ncnc2cc[nH]c12>CN(C=O)C>CCOC(=O)CCn1ccc2ncnc(Cl)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ae28bb6c867541d29f3282c7a18ac86e
CS(=O)(=O)CCN.O=C(O)CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>CS(=O)(=O)CCNC(=O)CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCC(=O)NCCS(=O)(=O)C.O.ON1N=NC2=C1C=CC=C2.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCC(=O)O.CS(=O)(=O)CCN.Cl.CN(CCCN=C=NCC)C.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCC(=O)NCCS(=O)(=O)C.Cl.C(C)(=O)OCC>>Cl.ClC=1C=C(C=CC1OC1=CC(=CC=...
[CH3:1][S:2](=[O:3])(=[O:4])[CH2:5][CH2:6][NH2:7].O[C:8](=[O:9])[CH2:10][CH2:11][n:12]1[cH:13][cH:14][c:15]2[n:16][cH:17][n:18][c:19]([NH:20][c:21]3[cH:22][cH:23][c:24]([O:25][c:26]4[cH:27][cH:28][cH:29][c:30]([C:31]([F:32])([F:33])[F:34])[cH:35]4)[c:36]([Cl:37])[cH:38]3)[c:39]12>>[CH3:1][S:2](=[O:3])(=[O:4])[CH2:5][CH...
CS(=O)(=O)CCN.O=C(O)CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
CS(=O)(=O)CCNC(=O)CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:7]-[C:6]-[C:5]
160
[{"value": 160.0, "product": "Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCC(=O)NCCS(=O)(=O)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
3-[4-({3-Chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]-N-[2-(methylsulfonyl)ethyl]propanamide (140 mg) was obtained by the reaction in the same manner as in Example 202 (iii) using 3-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]propanoic...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HO-
C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
null
null
CS(=O)(=O)CCN.O=C(O)CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC>CS(=O)(=O)CCNC(=O)CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b1eeedc5680c4a4cb7c99964c406f5af
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(OC(F)(F)F)c4)c(Cl)c3)c21>>O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(OC(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)OC(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CCO)=O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)OC(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CCO)=O.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)OC(F)(F)F)Cl.O.ON1N=NC2=C1C=CC=C2.OCCC(=O)O.Cl.C(C)(=O)OCC>>Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)OC(F)(F)F)NC=1C2=C(N=CN1)C=CN2CC...
[O:2]=[C:3]([CH2:4][CH2:5][OH:6])[NH:7][CH2:8][CH2:9][n:10]1[cH:11][cH:12][c:13]2[n:14][cH:15][n:16][c:17]([NH:18][c:19]3[cH:20][cH:21][c:22]([O:23][c:24]4[cH:25][cH:26][cH:27][c:28]([O:29][C:30]([F:31])([F:32])[F:33])[cH:34]4)[c:35]([Cl:36])[cH:37]3)[c:38]12>>[O:2]=[C:3]([CH2:4][CH2:5][OH:6])[NH:7][CH2:8][CH2:9][n:10]...
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(OC(F)(F)F)c4)c(Cl)c3)c21
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(OC(F)(F)F)c4)c(Cl)c3)c21
null
null
C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
null
null
[]
null
null
null
null
N-{2-[4-({3-Chloro-4-[3-(trifluoromethoxy)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxypropanamide was obtained by the reaction in the same manner as in Example 202 (iii) using 5-(2-aminoethyl)-N-{3-chloro-4-[3-(trifluoromethoxy)phenoxy]phenyl}-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
null
C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
null
null
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(OC(F)(F)F)c4)c(Cl)c3)c21>C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC>O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(OC(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-727036fe3ce147629a7effcd602129c3
COC(C)(C)OC.OCCCC(O)CO>>CC1(C)OCC(CCCO)O1
C(C(CCCO)O)O.COC(C)(C)OC.CC1=CC=C(C=C1)S(=O)(=O)O>>CC1(OCC(O1)CCCO)C
CO[C:2](OC)([CH3:1])[CH3:3].[OH:4][CH2:5][CH:6]([CH2:7][CH2:8][CH2:9][OH:10])[OH:11]>>[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][CH:6]([CH2:7][CH2:8][CH2:9][OH:10])[O:11]1
COC(C)(C)OC.OCCCC(O)CO
CC1(C)OCC(CCCO)O1
null
null
CC(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
64a00cd18ce80dbb6557ba4f70bb2bb92710e160014dcc8e9d84f6ab91dcc2c7
d3cf88dd21c2b1133a535341fad8736ebfcb343cc20bb0a78301ecc79ada442a
C1COCO1
C-O-[C;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-O-C.[C:4]-[C:5](-[OH;D1;+0:6])-[C:7]-[OH;D1;+0:8]>>[C:4]-[C:5]1-[C:7]-[O;H0;D2;+0:8]-[C;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[O;H0;D2;+0:6]-1
null
[]
null
null
1.5
HOUR
Pentane-1,2,5-triol (5.00 g) was dissolved in acetone (150 mL), 2,2-dimethoxypropane (10.5 mL) and 4-methylbenzenesulfonic acid (794 mg) were added, and the mixture was stirred at room temperature for 1.5 hrs. The reaction mixture was concentrated under reduced pressure, and the residue was separated and purified by si...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary alcohol.Secondary alcohol
Ether.Ether
null
C1COCO1
C1COCO1
HO-
CC(=O)C
null
1.5
COC(C)(C)OC.OCCCC(O)CO>CC(=O)C>CC1(C)OCC(CCCO)O1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-6b75f8e57f0542bcb32a489ef2dbd232
CC1(C)OCC(CCCn2ccc3ncnc(Cl)c32)O1.Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1>>OCC(O)CCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C2=C(N=CN1)C=CN2CCCC2OC(OC2)(C)C.ClC=1C=C(N)C=CC1OC1=CC(=CC=C1)C(F)(F)F.Cl.[OH-].[Na+]>>ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCCC(CO)O
CC1(C)[O:1][CH2:2][CH:3]([CH2:5][CH2:6][CH2:7][n:8]2[cH:9][cH:10][c:11]3[n:12][cH:13][n:14][c:15](Cl)[c:35]23)[O:4]1.[NH2:16][c:17]1[cH:18][cH:19][c:20]([O:21][c:22]2[cH:23][cH:24][cH:25][c:26]([C:27]([F:28])([F:29])[F:30])[cH:31]2)[c:32]([Cl:33])[cH:34]1>>[OH:1][CH2:2][CH:3]([OH:4])[CH2:5][CH2:6][CH2:7][n:8]1[cH:9][cH...
CC1(C)OCC(CCCn2ccc3ncnc(Cl)c32)O1.Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1
OCC(O)CCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
C(C)(C)O.CO
Heteroatom Alkylation and Arylation
OtherReaction
778e2670924c0ed8bcf6a90c6555a3540830d12c5cbfae1b13f74f1cc5382918
abf0b0ec18be67ff8c5cd168fe879220d788f51a7bacd61152dfeff2c16efa42
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
C-C1(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3](-[C:4])-[O;H0;D2;+0:5]-1.Cl-[c;H0;D3;+0:6]1:[#7;a:7]:[c:8]:[#7;a:9]:[c:10]2:[c:11]:[c:12]:[#7;a:13](-[C:14]):[c:15]:2:1.[NH2;D1;+0:16]-[c:17](:[c:18]):[c:19]>>[C:14]-[#7;a:13]1:[c:12]:[c:11]:[c:10]2:[#7;a:9]:[c:8]:[#7;a:7]:[c;H0;D3;+0:6](-[NH;D2;+0:16]-[c:17](:[c:18]):[c:19]):[c:15]:...
61.1
[{"value": 61.1, "product": "ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCCC(CO)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3.5
HOUR
The crude product was obtained by the reaction in the same manner as in Example 201 (iii) using 4-chloro-5-[3-(2,2-dimethyl-1,3-dioxolan-4-yl)propyl]-5H-pyrrolo[3,2-d]pyrimidine (171 mg), 3-chloro-4-[3-(trifluoromethyl)phenoxy]aniline (195 mg) and isopropyl alcohol (3.5 mL). The crude product was dissolved in methanol ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ether.Ether.Primary amine
Primary alcohol.Secondary alcohol.Secondary amine
C1COCO1.c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HCl
C(C)(C)O.CO
null
3.5
CC1(C)OCC(CCCn2ccc3ncnc(Cl)c32)O1.Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1>C(C)(C)O.CO>OCC(O)CCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3be30a51c2174b4691e184d20740a5a4
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CCO)=O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CCO)=O.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl.O.ON1N=NC2=C1C=CC=C2.OCCC(=O)O.Cl.C(C)(=O)OCC>>Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(C...
[O:2]=[C:3]([CH2:4][CH2:5][OH:6])[NH:7][CH2:8][CH2:9][n:10]1[cH:11][cH:12][c:13]2[n:14][cH:15][n:16][c:17]([NH:18][c:19]3[cH:20][cH:21][c:22]([O:23][c:24]4[cH:25][cH:26][cH:27][c:28]([C:29]([F:30])([F:31])[F:32])[cH:33]4)[c:34]([Cl:35])[cH:36]3)[c:37]12>>[O:2]=[C:3]([CH2:4][CH2:5][OH:6])[NH:7][CH2:8][CH2:9][n:10]1[cH:1...
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
null
null
[]
null
null
null
null
N-{2-[4-({3-Chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxypropanamide was obtained by the reaction in the same manner as in Example 202 (iii) using 5-(2-aminoethyl)-N-{3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride (...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
null
C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
null
null
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC>O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-aac7ad5b237b4d34a24963f4d259c78f
CC(C)(C)[Si](C)(C)OCCBr.CC1(C)OCC(CO)O1>>CC1(C)OCC(COCCO[Si](C)(C)C(C)(C)C)O1
[Cl-].[NH4+].[H-].[Na+].CC1(OCC(O1)CO)C.BrCCO[Si](C)(C)C(C)(C)C>>C(C)(C)(C)[Si](C)(C)OCCOCC1OC(OC1)(C)C
Br[CH2:9][CH2:10][O:11][Si:12]([CH3:13])([CH3:14])[C:15]([CH3:16])([CH3:17])[CH3:18].[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][CH:6]([CH2:7][OH:8])[O:19]1>>[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][CH:6]([CH2:7][O:8][CH2:9][CH2:10][O:11][Si:12]([CH3:13])([CH3:14])[C:15]([CH3:16])([CH3:17])[CH3:18])[O:19]1
CC(C)(C)[Si](C)(C)OCCBr.CC1(C)OCC(CO)O1
CC1(C)OCC(COCCO[Si](C)(C)C(C)(C)C)O1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
dd3f9c60e1f90d961a7c01d970ae213561355ee1451f276a3b04696e4b6fae5c
46a6e883cf919b4006e69abfdfd883f458f55c08b3200960c6a5b57c4139fbca
C1COCO1
Br-[CH2;D2;+0:1]-[C:2]-[#8:3].[#8:4]-[C:5]-[C:6]-[OH;D1;+0:7]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[O;H0;D2;+0:7]-[C:6]-[C:5]-[#8:4]
null
[]
0
CELSIUS
1
HOUR
60% Sodium hydride (890 mg) was suspended in N,N-dimethylformamide (60 mL), and the suspension was cooled to 0° C. (2,2-Dimethyl-1,3-dioxolan-4-yl)methanol (2.3 mL) was added dropwise and the mixture was stirred at 0° C. for 1 hr. To the reaction mixture was added (2-bromoethoxy)(tert-butyl)dimethylsilane (3 mL), and t...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary alcohol
Ether
null
null
C1COCO1
HBr
CN(C=O)C
0
1
CC(C)(C)[Si](C)(C)OCCBr.CC1(C)OCC(CO)O1>CN(C=O)C>CC1(C)OCC(COCCO[Si](C)(C)C(C)(C)C)O1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-38e0377754744a099ec489544f1e7272
CC1(C)OCC(COCCO[Si](C)(C)C(C)(C)C)O1.CS(=O)(=O)Cl>>CC1(C)OCC(COCCOS(C)(=O)=O)O1
[Cl-].[NH4+].[F-].C(CCC)[N+](CCCC)(CCCC)CCCC.C(C)(C)(C)[Si](C)(C)OCCOCC1OC(OC1)(C)C.CS(=O)(=O)Cl>>CS(=O)(=O)OCCOCC1OC(OC1)(C)C
CC(C)(C)[Si](C)(C)[O:11][CH2:10][CH2:9][O:8][CH2:7][CH:6]1[CH2:5][O:4][C:2]([CH3:1])([CH3:3])[O:16]1.Cl[S:12]([CH3:13])(=[O:14])=[O:15]>>[CH3:1][C:2]1([CH3:3])[O:4][CH2:5][CH:6]([CH2:7][O:8][CH2:9][CH2:10][O:11][S:12]([CH3:13])(=[O:14])=[O:15])[O:16]1
CC1(C)OCC(COCCO[Si](C)(C)C(C)(C)C)O1.CS(=O)(=O)Cl
CC1(C)OCC(COCCOS(C)(=O)=O)O1
null
null
O1CCCC1.C(C)N(CC)CC
Acylation
Formation of Sulfonic Esters on TMS protected alcohol
9e07f5520b3bc5500a9061296fe6119923fb94fe35985540b2063263d581dc98
acebbce8dd2300bebe4cae2d4fdddc23ab537bab21f7d9c9767166502cc48828
C1COCO1
C-C(-C)(-C)-[Si](-C)(-C)-[O;H0;D2;+0:1]-[C:2]-[C:3].Cl-[S;H0;D4;+0:4](-[C;D1;H3:5])(=[O;D1;H0:6])=[O;D1;H0:7]>>[C:3]-[C:2]-[O;H0;D2;+0:1]-[S;H0;D4;+0:4](-[C;D1;H3:5])(=[O;D1;H0:6])=[O;D1;H0:7]
null
[]
null
null
1
HOUR
tert-Butyl{2-[(2,2-dimethyl-1,3-dioxolan-4-yl)methoxy]ethoxy}dimethylsilane (1.03 g) was dissolved in tetrahydrofuran (20 mL), a 1.0 M solution (4 mL) of tetrabutylammonium fluoride in tetrahydrofuran was added, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added saturated aqueou...
10.6084/m9.figshare.5104873.v1
null
Sulfonyl halide.TMS ether protective group
Mesylate
null
null
C1COCO1
HCl
O1CCCC1.C(C)N(CC)CC
null
1
CC1(C)OCC(COCCO[Si](C)(C)C(C)(C)C)O1.CS(=O)(=O)Cl>O1CCCC1.C(C)N(CC)CC>CC1(C)OCC(COCCOS(C)(=O)=O)O1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-66ccf0905d1247ef9bb07dee9ad0924b
Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1.OCC(O)COCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>OCC(O)COCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCOCC(CO)O.ClC=1C2=C(N=CN1)C=CN2CCOCC2OC(OC2)(C)C.ClC=1C=C(N)C=CC1OC1=CC(=CC=C1)C(F)(F)F.Cl.C(C)(=O)OCC.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCOCC(CO)O>>Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCOCC(CO)O
[NH2:18][c:19]1[cH:20][cH:21][c:22]([O:23][c:24]2[cH:25][cH:26][cH:27][c:28]([C:29]([F:30])([F:31])[F:32])[cH:33]2)[c:34]([Cl:35])[cH:36]1.FC(F)(F)c1cccc(Oc2ccc(N[c:17]3[n:16][cH:15][n:14][c:13]4[cH:12][cH:11][n:10]([CH2:9][CH2:8][O:7][CH2:6][CH:4]([CH2:3][OH:2])[OH:5])[c:37]43)cc2Cl)c1>>[OH:2][CH2:3][CH:4]([OH:5])[CH2...
Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1.OCC(O)COCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
OCC(O)COCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
C(C)(C)O.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
e88e7a61524392eb0cb258a4f882c1cc83f2511cff5bd223c6ff56dc8d10ae74
ed0de786cbeaa40aae734f133871c22959d29ff35283ad441d3d1e171aa960b7
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
Cl-c1:c:c(-N-[c;H0;D3;+0:1]2:[#7;a:2]:[c:3]:[#7;a:4]:[c:5]3:[c:6]:[c:7]:[#7;a:8](-[C:9]):[c:10]:3:2):c:c:c:1-O-c1:c:c:c:c(-C(-F)(-F)-F):c:1.[NH2;D1;+0:11]-[c:12](:[c:13]):[c:14]>>[C:9]-[#7;a:8]1:[c:7]:[c:6]:[c:5]2:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:11]-[c:12](:[c:13]):[c:14]):[c:10]:1:2
null
[]
null
null
null
null
3-{2-[4-({3-Chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethoxy}propane-1,2-diol was obtained by the reaction in the same manner as in Example 237 (iv) using 4-chloro-5-{2-[(2,2-dimethyl-1,3-dioxolan-4-yl)methoxy]ethyl}-5H-pyrrolo[3,2-d]pyrimidine (295 mg), 3-chloro-4-[3-(trifluoro...
10.6084/m9.figshare.5104873.v1
null
Trifluoro group.Aromatic halide.Ether.Primary amine.Secondary amine
Secondary amine
c1ccccc1.c1ccccc1.c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HF
C(C)(C)O.C(C)(=O)OCC
null
null
Nc1ccc(Oc2cccc(C(F)(F)F)c2)c(Cl)c1.OCC(O)COCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>C(C)(C)O.C(C)(=O)OCC>OCC(O)COCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-13b49d39009f45fd8c49f218ee7219ad
CC(C)(C)OC(=O)NCC#CCCl.Clc1ncnc2cc[nH]c12>>CC(C)(C)OC(=O)NCC#CCn1ccc2ncnc(Cl)c21
ClC=1C2=C(N=CN1)C=CN2.ClCC#CCNC(OC(C)(C)C)=O.C([O-])([O-])=O.[Cs+].[Cs+].CN(C=O)C>>C(C)(C)(C)OC(NCC#CCN1C=CC=2N=CN=C(C21)Cl)=O
Cl[CH2:12][C:11]#[C:10][CH2:9][NH:8][C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7].[nH:13]1[cH:14][cH:15][c:16]2[n:17][cH:18][n:19][c:20]([Cl:21])[c:22]12>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[NH:8][CH2:9][C:10]#[C:11][CH2:12][n:13]1[cH:14][cH:15][c:16]2[n:17][cH:18][n:19][c:20]([Cl:21])[c:22]12
CC(C)(C)OC(=O)NCC#CCCl.Clc1ncnc2cc[nH]c12
CC(C)(C)OC(=O)NCC#CCn1ccc2ncnc(Cl)c21
null
null
O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
ecfdd3ebe7f504d096c44af08936ff56b52d45d78f82ef9c3a3c3047f20010b5
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
c1ncc2[nH]ccc2n1
Cl-[CH2;D2;+0:1]-[C:2]#[C:3]-[C:4].[Cl;D1;H0:5]-[c:6]1:[#7;a:7]:[c:8]:[#7;a:9]:[c:10]2:[c:11]:[c:12]:[nH;D2;+0:13]:[c:14]:2:1>>[C:4]-[C:3]#[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:13]1:[c:12]:[c:11]:[c:10]2:[#7;a:9]:[c:8]:[#7;a:7]:[c:6](-[Cl;D1;H0:5]):[c:14]:2:1
82.8
[{"value": 82.8, "product": "C(C)(C)(C)OC(NCC#CCN1C=CC=2N=CN=C(C21)Cl)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A mixture of 4-chloro-5H-pyrrolo[3,2-d]pyrimidine (1.51 g), tert-butyl (4-chlorobut-2-yn-1-yl)carbamate (2.60 g), cesium carbonate (4.80 g) and N,N-dimethylformamide (15 mL) was stirred at room temperature for 2 hrs. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic l...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1ncc2[nH]ccc2n1
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
HCl
O
null
2
CC(C)(C)OC(=O)NCC#CCCl.Clc1ncnc2cc[nH]c12>O>CC(C)(C)OC(=O)NCC#CCn1ccc2ncnc(Cl)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9f6364c434794bd183abe416a1e7c9f7
CC(C)(C)OC(=O)NCC#CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>Cl.NCC#CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CC#CCNC(OC(C)(C)C)=O.Cl.C(C)O>>Cl.Cl.NCC#CCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl
CC(C)(C)OC(=O)[NH:3][CH2:4][C:5]#[C:6][CH2:7][n:8]1[cH:9][cH:10][c:11]2[n:12][cH:13][n:14][c:15]([NH:16][c:17]3[cH:18][cH:19][c:20]([O:21][c:22]4[cH:23][cH:24][cH:25][c:26]([C:27]([F:28])([F:29])[F:30])[cH:31]4)[c:32]([Cl:2])[cH:34]3)[c:35]12>>[ClH:2].[NH2:3][CH2:4][C:5]#[C:6][CH2:7][n:8]1[cH:9][cH:10][c:11]2[n:12][cH:...
CC(C)(C)OC(=O)NCC#CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
Cl.NCC#CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
O1CCCC1
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
f9b0ddd5e086b40f0768881f9b226acdc5a9dc29f99a9283af567e925b55a3d7
b15a28c2a3fd58b98c3a6c1b435f8c25519aeb02339cc9ac8ff8fecd35099d5c
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]#[C:4]-[C:5].[#8:6]-[c:7](:[c:8]):[c;H0;D3;+0:9](-[Cl;H0;D1;+0:10]):[c:11]:[c:12]>>[#8:6]-[c:7](:[c:8]):[c;H0;D3;+0:9](-[Cl;D1;H0:13]):[c:11]:[c:12].[C:5]-[C:4]#[C:3]-[C:2]-[NH2;D1;+0:1].[ClH;D0;+0:10]
null
[]
60
CELSIUS
16
HOUR
tert-Butyl {4-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]but-2-yn-1-yl}carbamate (1.90 g) was dissolved in tetrahydrofuran (35 mL), 2N hydrochloric acid (18 mL) was added, and the mixture was stirred at 60° C. for 16 hrs. To the reaction mixture was added ethanol, and the ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Boc
Aromatic halide.Primary amine
c1ccccc1
c1ccccc1
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HO-
O1CCCC1
60
16
CC(C)(C)OC(=O)NCC#CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>O1CCCC1>Cl.NCC#CCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3089ba9acaa543c69e2a13e4bc2e376d
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CCO)=O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(CCO)=O.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl.O.ON1N=NC2=C1C=CC=C2.OCCC(=O)O.CS(=O)(=O)O>>CS(=O)(=O)O.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2...
[O:6]=[C:7]([CH2:8][CH2:9][OH:10])[NH:11][CH2:12][CH2:13][n:14]1[cH:15][cH:16][c:17]2[n:18][cH:19][n:20][c:21]([NH:22][c:23]3[cH:24][cH:25][c:26]([O:27][c:28]4[cH:29][cH:30][cH:31][c:32]([C:33]([F:34])([F:35])[F:36])[cH:37]4)[c:38]([Cl:39])[cH:40]3)[c:41]12>>[O:6]=[C:7]([CH2:8][CH2:9][OH:10])[NH:11][CH2:12][CH2:13][n:1...
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
null
null
O1CCCC1.C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
null
null
[]
null
null
2
HOUR
N-{2-[4-({3-Chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-3-hydroxypropanamide was obtained by the reaction in the same manner as in Example 202 (iii) using 5-(2-aminoethyl)-N-{3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride (...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
null
O1CCCC1.C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC
null
2
O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>O1CCCC1.C(C)N(CC)CC.CN(C=O)C.C(C)(=O)OCC>O=C(CCO)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-43d1bb55d14042ebbcf28587c74083bd
Cc1cc(Nc2ncnc3ccn(CCNC(=O)OC(C)(C)C)c23)ccc1Oc1cccc(C(F)(F)F)c1>>Cc1cc(Nc2ncnc3ccn(CCN)c23)ccc1Oc1cccc(C(F)(F)F)c1.Cl
CC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(OC(C)(C)C)=O.Cl>>Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)C
CC(C)(C)OC(=O)[NH:16][CH2:15][CH2:14][n:13]1[cH:12][cH:11][c:10]2[n:9][cH:8][n:7][c:6]([NH:5][c:4]3[cH:3][c:2]([CH3:1])[c:20]([O:21][c:22]4[cH:23][cH:24][cH:25][c:26]([C:27]([F:28])([F:29])[F:30])[cH:31]4)[cH:19][cH:18]3)[c:17]21>>[CH3:1][c:2]1[cH:3][c:4]([NH:5][c:6]2[n:7][cH:8][n:9][c:10]3[cH:11][cH:12][n:13]([CH2:14]...
Cc1cc(Nc2ncnc3ccn(CCNC(=O)OC(C)(C)C)c23)ccc1Oc1cccc(C(F)(F)F)c1
Cc1cc(Nc2ncnc3ccn(CCN)c23)ccc1Oc1cccc(C(F)(F)F)c1.Cl
null
null
O1CCCC1
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
4812e39fa209f57a5a2564677791e5e37790c829f5742d8c7df33806c5ba4ce0
d7ecc2e7a68b8c20d378ac6004c3fdfc3efd09bbbd9efd577186f69427135737
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
60
CELSIUS
16
HOUR
tert-Butyl {2-[4-({3-methyl-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}carbamate (2.9 g) obtained in Example 188 (i) was dissolved in tetrahydrofuran (80 mL)/2N hydrochloric acid (40 mL), and the mixture was stirred at 60° C. for 16 hrs. The reaction mixture was concentrated under...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ncnc2cc[nH]c12.c1ccccc1
HO-
O1CCCC1
60
16
Cc1cc(Nc2ncnc3ccn(CCNC(=O)OC(C)(C)C)c23)ccc1Oc1cccc(C(F)(F)F)c1>O1CCCC1>Cc1cc(Nc2ncnc3ccn(CCN)c23)ccc1Oc1cccc(C(F)(F)F)c1.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-066edf0fe8774d78b4e156b207fb64dd
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCNC(=O)OC(C)(C)C)c34)cc2C)cn1>>Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCN)c34)cc2C)cn1.Cl.Cl
CC=1C=C(C=CC1OC=1C=NC(=CC1)C)NC=1C2=C(N=CN1)C=CN2CCNC(OC(C)(C)C)=O.Cl>>Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC=2C=NC(=CC2)C)C
CC(C)(C)OC(=O)[NH:22][CH2:21][CH2:20][n:19]1[cH:18][cH:17][c:16]2[n:15][cH:14][n:13][c:12]([NH:11][c:10]3[cH:9][cH:8][c:7]([O:6][c:5]4[cH:4][cH:3][c:2]([CH3:1])[n:28][cH:27]4)[c:25]([CH3:26])[cH:24]3)[c:23]21>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([O:6][c:7]2[cH:8][cH:9][c:10]([NH:11][c:12]3[n:13][cH:14][n:15][c:16]4[cH:17][c...
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCNC(=O)OC(C)(C)C)c34)cc2C)cn1
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCN)c34)cc2C)cn1.Cl.Cl
null
null
O1CCCC1
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
4812e39fa209f57a5a2564677791e5e37790c829f5742d8c7df33806c5ba4ce0
d7ecc2e7a68b8c20d378ac6004c3fdfc3efd09bbbd9efd577186f69427135737
c1cncc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
null
[]
60
CELSIUS
16
HOUR
tert-Butyl {2-[4-({3-methyl-4-[(6-methylpyridin-3-yl)oxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}carbamate (790 mg) was dissolved in tetrahydrofuran (24 mL)/2N hydrochloric acid (12 mL), and the mixture was stirred at 60° C. for 16 hrs. The reaction mixture was concentrated under reduced pressure, ethanol (...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccncc1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O1CCCC1
60
16
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCNC(=O)OC(C)(C)C)c34)cc2C)cn1>O1CCCC1>Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCN)c34)cc2C)cn1.Cl.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c1ac56260547463faad1b51a844aa013
CC(C)(C)OC(=O)NCCn1ccc2ncnc(Nc3ccc(OCc4ccccn4)c(Cl)c3)c21>>Cl.Cl.Cl.NCCn1ccc2ncnc(Nc3ccc(OCc4ccccn4)c(Cl)c3)c21
C(C)(C)(C)OC(NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OCC2=NC=CC=C2)Cl)=O>>Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OCC2=NC=CC=C2)Cl
CC(C)(C)OC(=O)[NH:4][CH2:5][CH2:6][n:7]1[cH:8][cH:9][c:10]2[n:11][cH:12][n:13][c:14]([NH:15][c:16]3[cH:17][cH:18][c:19]([O:20][CH2:21][c:22]4[cH:23][cH:24][cH:25][cH:26][n:27]4)[c:28]([Cl:1])[cH:30]3)[c:31]12>>[ClH:1].[ClH:2].[ClH:3].[NH2:4][CH2:5][CH2:6][n:7]1[cH:8][cH:9][c:10]2[n:11][cH:12][n:13][c:14]([NH:15][c:16]3...
CC(C)(C)OC(=O)NCCn1ccc2ncnc(Nc3ccc(OCc4ccccn4)c(Cl)c3)c21
Cl.Cl.Cl.NCCn1ccc2ncnc(Nc3ccc(OCc4ccccn4)c(Cl)c3)c21
null
null
O1CCCC1.Cl
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
f9b0ddd5e086b40f0768881f9b226acdc5a9dc29f99a9283af567e925b55a3d7
b15a28c2a3fd58b98c3a6c1b435f8c25519aeb02339cc9ac8ff8fecd35099d5c
c1ccc(COc2ccc(Nc3ncnc4cc[nH]c34)cc2)nc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3].[#8:4]-[c:5](:[c:6]):[c;H0;D3;+0:7](-[Cl;H0;D1;+0:8]):[c:9]:[c:10]>>[#8:4]-[c:5](:[c:6]):[c;H0;D3;+0:7](-[Cl;D1;H0:11]):[c:9]:[c:10].[C:3]-[C:2]-[NH2;D1;+0:1].[ClH;D0;+0:8]
410.5
[{"value": 410.5, "product": "Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OCC2=NC=CC=C2)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
16
HOUR
tert-Butyl[2-(4-{[3-chloro-4-(pyridin-2-ylmethoxy)phenyl]amino}-5H-pyrrolo[3,2-d]pyrimidin-5-yl)ethyl]carbamate (790 mg) was dissolved in tetrahydrofuran (24 mL)/2N hydrochloric acid (12 mL), and the mixture was stirred at 60° C. for 16 hrs. The reaction mixture was concentrated under reduced pressure, ethanol (30 mL) ...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Boc
Aromatic halide.Primary amine
c1ccccc1
c1ccccc1
c1ncnc2cc[nH]c12.c1ccccc1.c1ccncc1
HO-
O1CCCC1.Cl
60
16
CC(C)(C)OC(=O)NCCn1ccc2ncnc(Nc3ccc(OCc4ccccn4)c(Cl)c3)c21>O1CCCC1.Cl>Cl.Cl.Cl.NCCn1ccc2ncnc(Nc3ccc(OCc4ccccn4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8988d36cb8724375af4584acc9ac0193
Cc1cc(Nc2ncnc3ccn(CCNC(=O)[C@@H]4C[C@@H](O)CN4C(=O)OC(C)(C)C)c23)ccc1Oc1cccc(C(F)(F)F)c1.ClCCl>>Cc1cc(Nc2ncnc3ccn(CCNC(=O)[C@@H]4C[C@@H](O)CN4)c23)ccc1Oc1cccc(C(F)(F)F)c1.Cl.Cl
O[C@@H]1C[C@H](N(C1)C(=O)OC(C)(C)C)C(=O)NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)C.ClCCl.FC(C(=O)O)(F)F>>Cl.Cl.O[C@@H]1C[C@H](NC1)C(=O)NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)C
CC(C)(C)OC(=O)[N:24]1[C@H:19]([C:17]([NH:16][CH2:15][CH2:14][n:13]2[cH:12][cH:11][c:10]3[n:9][cH:8][n:7][c:6]([NH:5][c:4]4[cH:3][c:2]([CH3:1])[c:28]([O:29][c:30]5[cH:31][cH:32][cH:33][c:34]([C:35]([F:36])([F:37])[F:38])[cH:39]5)[cH:27][cH:26]4)[c:25]32)=[O:18])[CH2:20][C@@H:21]([OH:22])[CH2:23]1.C([Cl:40])[Cl:41]>>[CH3...
Cc1cc(Nc2ncnc3ccn(CCNC(=O)[C@@H]4C[C@@H](O)CN4C(=O)OC(C)(C)C)c23)ccc1Oc1cccc(C(F)(F)F)c1.ClCCl
Cc1cc(Nc2ncnc3ccn(CCNC(=O)[C@@H]4C[C@@H](O)CN4)c23)ccc1Oc1cccc(C(F)(F)F)c1.Cl.Cl
null
null
null
Miscellaneous
OtherReaction
3d13376f22099a603cf8d03ba2bae39027a371e34833ba8f6048c2d87eee4b71
016f034d4f383e2d40e897f441602a7d95bad94b528953d03d8a2ec434dca97e
O=C(NCCn1ccc2ncnc(Nc3ccc(Oc4ccccc4)cc3)c21)[C@@H]1CCCN1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1-[C:6](=[O;D1;H0:7])-[#7:8]-[C:9].[Cl;H0;D1;+0:10]-C-[Cl;H0;D1;+0:11]>>[C:9]-[#7:8]-[C:6](=[O;D1;H0:7])-[C:5]1-[C:4]-[C:3]-[C:2]-[NH;D2;+0:1]-1.[ClH;D0;+0:10].[ClH;D0;+0:11]
null
[]
null
null
2
HOUR
tert-Butyl (2S,4R)-4-hydroxy-2-[({2-[4-({3-methyl-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}amino)carbonyl]pyrrolidine-1-carboxylate (230 mg) was dissolved in dichloromethane (2.39 mL), trifluoroacetic acid (1.79 mL) was added, and the mixture was stirred at room temperature for ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Primary halide.Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]C1
C1CCNC1
c1ccccc1.c1ncnc2cc[nH]c12.C1CCNC1.c1ccccc1
HO-
null
null
2
Cc1cc(Nc2ncnc3ccn(CCNC(=O)[C@@H]4C[C@@H](O)CN4C(=O)OC(C)(C)C)c23)ccc1Oc1cccc(C(F)(F)F)c1.ClCCl>>Cc1cc(Nc2ncnc3ccn(CCNC(=O)[C@@H]4C[C@@H](O)CN4)c23)ccc1Oc1cccc(C(F)(F)F)c1.Cl.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1206b0d56e3440eb8baf39b4de1476e3
Cc1cc(Nc2ncnc3ccn(CCNC(=O)CS(C)(=O)=O)c23)ccc1Oc1cccc(C(F)(F)F)c1>>Cc1cc(Nc2ncnc3ccn(CCNC(=O)CS(C)(=O)=O)c23)ccc1Oc1cccc(C(F)(F)F)c1
CS(=O)(=O)CC(=O)NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)C.CS(=O)(=O)O>>CS(=O)(=O)O.CS(=O)(=O)CC(=O)NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)C
[CH3:6][c:7]1[cH:8][c:9]([NH:10][c:11]2[n:12][cH:13][n:14][c:15]3[cH:16][cH:17][n:18]([CH2:19][CH2:20][NH:21][C:22](=[O:23])[CH2:24][S:25]([CH3:26])(=[O:27])=[O:28])[c:29]23)[cH:30][cH:31][c:32]1[O:33][c:34]1[cH:35][cH:36][cH:37][c:38]([C:39]([F:40])([F:41])[F:42])[cH:43]1>>[CH3:6][c:7]1[cH:8][c:9]([NH:10][c:11]2[n:12]...
Cc1cc(Nc2ncnc3ccn(CCNC(=O)CS(C)(=O)=O)c23)ccc1Oc1cccc(C(F)(F)F)c1
Cc1cc(Nc2ncnc3ccn(CCNC(=O)CS(C)(=O)=O)c23)ccc1Oc1cccc(C(F)(F)F)c1
null
null
C(C)(=O)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
null
null
[]
null
null
10
MINUTE
2-(Methylsulfonyl)-N-{2-[4-({3-methyl-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}acetamide (680 mg) was dissolved in ethyl acetate (3.4 mL), methanesulfonic acid (0.0887 mL) was added at 50° C., and the mixture was stirred for 10 min. and further stirred at room temperature for 2 ...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ncnc2cc[nH]c12.c1ccccc1
null
C(C)(=O)OCC
null
0.166667
Cc1cc(Nc2ncnc3ccn(CCNC(=O)CS(C)(=O)=O)c23)ccc1Oc1cccc(C(F)(F)F)c1>C(C)(=O)OCC>Cc1cc(Nc2ncnc3ccn(CCNC(=O)CS(C)(=O)=O)c23)ccc1Oc1cccc(C(F)(F)F)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-739d42940f924f468639aa15c41653b5
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCNC(=O)OC(C)(C)C)c34)cc2Cl)cn1>>Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCN)c34)cc2Cl)cn1.Cl.Cl.Cl
ClC=1C=C(C=CC1OC=1C=NC(=CC1)C)NC=1C2=C(N=CN1)C=CN2CCNC(OC(C)(C)C)=O>>Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC=2C=NC(=CC2)C)Cl
CC(C)(C)OC(=O)[NH:22][CH2:21][CH2:20][n:19]1[cH:18][cH:17][c:16]2[n:15][cH:14][n:13][c:12]([NH:11][c:10]3[cH:9][cH:8][c:7]([O:6][c:5]4[cH:4][cH:3][c:2]([CH3:1])[n:28][cH:27]4)[c:25]([Cl:26])[cH:24]3)[c:23]21>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([O:6][c:7]2[cH:8][cH:9][c:10]([NH:11][c:12]3[n:13][cH:14][n:15][c:16]4[cH:17][cH...
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCNC(=O)OC(C)(C)C)c34)cc2Cl)cn1
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCN)c34)cc2Cl)cn1.Cl.Cl.Cl
null
null
O1CCCC1.Cl
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
4812e39fa209f57a5a2564677791e5e37790c829f5742d8c7df33806c5ba4ce0
d7ecc2e7a68b8c20d378ac6004c3fdfc3efd09bbbd9efd577186f69427135737
c1cncc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3]>>[C:3]-[C:2]-[NH2;D1;+0:1]
394.5
[{"value": 394.5, "product": "Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC=2C=NC(=CC2)C)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
16
HOUR
tert-Butyl {2-[4-({3-chloro-4-[(6-methylpyridin-3-yl)oxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}carbamate (643 mg) was dissolved in tetrahydrofuran (19.5 mL)/2N hydrochloric acid (9.75 mL), and the mixture was stirred at 60° C. for 16 hrs. The reaction mixture was concentrated under reduced pressure, ethan...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccncc1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O1CCCC1.Cl
60
16
Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCNC(=O)OC(C)(C)C)c34)cc2Cl)cn1>O1CCCC1.Cl>Cc1ccc(Oc2ccc(Nc3ncnc4ccn(CCN)c34)cc2Cl)cn1.Cl.Cl.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b25460c3526e400fbf67d72aa76ce5f2
CC(C)(C)OC(=O)NCCn1ccc2ncnc(Nc3ccc(Oc4cncc(Cl)c4)c(Cl)c3)c21>>Cl.Cl.Cl.NCCn1ccc2ncnc(Nc3ccc(Oc4cncc(Cl)c4)c(Cl)c3)c21
ClC=1C=C(C=CC1OC=1C=NC=C(C1)Cl)NC=1C2=C(N=CN1)C=CN2CCNC(OC(C)(C)C)=O>>Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC=2C=NC=C(C2)Cl)Cl
CC(C)(C)OC(=O)[NH:4][CH2:5][CH2:6][n:7]1[cH:8][cH:9][c:10]2[n:11][cH:12][n:13][c:14]([NH:15][c:16]3[cH:17][cH:18][c:19]([O:20][c:21]4[cH:22][n:23][cH:24][c:25]([Cl:26])[cH:27]4)[c:28]([Cl:1])[cH:30]3)[c:31]12>>[ClH:1].[ClH:2].[ClH:3].[NH2:4][CH2:5][CH2:6][n:7]1[cH:8][cH:9][c:10]2[n:11][cH:12][n:13][c:14]([NH:15][c:16]3...
CC(C)(C)OC(=O)NCCn1ccc2ncnc(Nc3ccc(Oc4cncc(Cl)c4)c(Cl)c3)c21
Cl.Cl.Cl.NCCn1ccc2ncnc(Nc3ccc(Oc4cncc(Cl)c4)c(Cl)c3)c21
null
null
O1CCCC1.Cl
Miscellaneous
Hydrogenolysis of amides/imides/carbamates
f9b0ddd5e086b40f0768881f9b226acdc5a9dc29f99a9283af567e925b55a3d7
b15a28c2a3fd58b98c3a6c1b435f8c25519aeb02339cc9ac8ff8fecd35099d5c
c1cncc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)c1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2]-[C:3].[#8:4]-[c:5](:[c:6]):[c;H0;D3;+0:7](-[Cl;H0;D1;+0:8]):[c:9]:[c:10]>>[#8:4]-[c:5](:[c:6]):[c;H0;D3;+0:7](-[Cl;D1;H0:11]):[c:9]:[c:10].[C:3]-[C:2]-[NH2;D1;+0:1].[ClH;D0;+0:8]
372.2
[{"value": 372.2, "product": "Cl.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC=2C=NC=C(C2)Cl)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
16
HOUR
tert-Butyl {2-[4-({3-chloro-4-[(5-chloropyridin-3-yl)oxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}carbamate (700 mg) was dissolved in tetrahydrofuran (19.5 mL)/2N hydrochloric acid (9.75 mL), and the mixture was stirred at 60° C. for 16 hrs. The reaction mixture was concentrated under reduced pressure, ethan...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Boc
Aromatic halide.Primary amine
c1ccccc1
c1ccccc1
c1ncnc2cc[nH]c12.c1ccccc1.c1ccncc1
HO-
O1CCCC1.Cl
60
16
CC(C)(C)OC(=O)NCCn1ccc2ncnc(Nc3ccc(Oc4cncc(Cl)c4)c(Cl)c3)c21>O1CCCC1.Cl>Cl.Cl.Cl.NCCn1ccc2ncnc(Nc3ccc(Oc4cncc(Cl)c4)c(Cl)c3)c21
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-8a447af30e9f43128ca371e783d545cd
CC(C)(C)OC(=O)N1CCC(Oc2ccc(N)cc2Cl)CC1.O=C(OCCOCCn1ccc2ncnc(Cl)c21)c1ccccc1>>CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1
C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)Cl.NC1=CC(=C(OC2CCN(CC2)C(=O)OC(C)(C)C)C=C1)Cl>>C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1CCN(CC1)C(=O)OC(C)(C)C)C=C2)Cl
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([O:12][c:13]2[cH:14][cH:15][c:16]([NH2:17])[cH:41][c:42]2[Cl:43])[CH2:44][CH2:45]1.Cl[c:18]1[n:19][cH:20][n:21][c:22]2[cH:23][cH:24][n:25]([CH2:26][CH2:27][O:28][CH2:29][CH2:30][O:31][C:32](=[O:33])[c:34]3[cH:35][cH:36][cH:37][cH:38][cH:39]3)[...
CC(C)(C)OC(=O)N1CCC(Oc2ccc(N)cc2Cl)CC1.O=C(OCCOCCn1ccc2ncnc(Cl)c21)c1ccccc1
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1
null
null
C(C)(C)O
Heteroatom Alkylation and Arylation
Goldberg coupling aryl amine-aryl chloride
b3e82b6ead9cdf4e2f8cbbcf91109747f4dd1119eb8fb5a3a7a9710387d7d6e5
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)cc3)c21)c1ccccc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5]2:[c:6]:[c:7]:[#7;a:8](-[C:9]):[c:10]:2:1.[NH2;D1;+0:11]-[c:12](:[c:13]):[c:14]>>[C:9]-[#7;a:8]1:[c:7]:[c:6]:[c:5]2:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:11]-[c:12](:[c:13]):[c:14]):[c:10]:1:2
73.8
[{"value": 73.8, "product": "C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1CCN(CC1)C(=O)OC(C)(C)C)C=C2)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
8
HOUR
A mixture of 2-[2-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-5-yl)ethoxy]ethyl benzoate (3.46 g), tert-butyl 4-(4-amino-2-chlorophenoxy)piperidine-1-carboxylate (3.27 g) and isopropyl alcohol (50 mL) was stirred at 80° C. overnight. The reaction mixture was concentrated under reduced pressure, water and saturated aqueous sod...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
C1CC[NH]CC1.c1ccccc1.c1ncnc2cc[nH]c12.c1ccccc1
HCl
C(C)(C)O
80
8
CC(C)(C)OC(=O)N1CCC(Oc2ccc(N)cc2Cl)CC1.O=C(OCCOCCn1ccc2ncnc(Cl)c21)c1ccccc1>C(C)(C)O>CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3559578cd4894683bf480130268e4df3
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1>>CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1CCN(CC1)C(=O)OC(C)(C)C)C=C2)Cl.O>>ClC1=C(OC2CCN(CC2)C(=O)OC(C)(C)C)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO
O=C(c1ccccc1)[O:31][CH2:30][CH2:29][O:28][CH2:27][CH2:26][n:25]1[cH:24][cH:23][c:22]2[n:21][cH:20][n:19][c:18]([NH:17][c:16]3[cH:15][cH:14][c:13]([O:12][CH:11]4[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:37][CH2:36]4)[c:34]([Cl:35])[cH:33]3)[c:32]21>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:...
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
null
null
O1CCCC1.CO.[OH-].[Na+]
Reduction
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
8df1b5c4ec88eb8f4e334a9ade2ac7fc0b3f460ea1450816d1758f28eee39662
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1nc(Nc2ccc(OC3CCNCC3)cc2)c2[nH]ccc2n1
O=C(-[O;H0;D2;+0:1]-[C:2]-[C:3])-c1:c:c:c:c:c:1>>[C:3]-[C:2]-[OH;D1;+0:1]
93.6
[{"value": 93.6, "product": "ClC1=C(OC2CCN(CC2)C(=O)OC(C)(C)C)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
tert-Butyl 4-{4-[(5-{2-[2-(benzoyloxy)ethoxy]ethyl}-5H-pyrrolo[3,2-d]pyrimidin-4-yl)amino]-2-chlorophenoxy}piperidine-1-carboxylate (636 mg) was dissolved in a mixed solvent of methanol (10 mL) and tetrahydrofuran (10 mL), 1N aqueous sodium hydroxide solution (2 mL) was added, and the mixture was stirred overnight at r...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
c1ccccc1
null
C1CC[NH]CC1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O1CCCC1.CO.[OH-].[Na+]
null
8
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1>O1CCCC1.CO.[OH-].[Na+]>CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-61723fdf027b4fffbd014f52b48ec0c5
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1>>Cl.O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1
Cl.C(C)(=O)OCC.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1CCN(CC1)C(=O)OC(C)(C)C)C=C2)Cl>>Cl.Cl.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2CCNCC2)Cl
CC(C)(C)OC(=O)[N:28]1[CH2:27][CH2:26][CH:25]([O:24][c:23]2[cH:22][cH:21][c:20]([NH:19][c:18]3[n:17][cH:16][n:15][c:14]4[cH:13][cH:12][n:11]([CH2:10][CH2:9][O:8][CH2:7][CH2:6][O:5][C:4](=[O:3])[c:35]5[cH:36][cH:37][cH:38][cH:39][cH:40]5)[c:34]43)[cH:33][c:31]2[Cl:1])[CH2:30][CH2:29]1>>[ClH:1].[O:3]=[C:4]([O:5][CH2:6][CH...
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1
Cl.O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1
null
null
C(C)O
Miscellaneous
Boc amine deprotection
ce4c3ea9d0c2faff3b9f7452f75b24d2d30bf40e954020ffa8aa94c1924df770
8eaac4d88ccfd676cb152ac8731ddb039e8a75c2631f9792b0a36d78d07a9740
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)cc3)c21)c1ccccc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5].[#8:6]-[c:7](:[c:8]):[c;H0;D3;+0:9](-[Cl;H0;D1;+0:10]):[c:11]:[c:12]>>[#8:6]-[c:7](:[c:8]):[c;H0;D3;+0:9](-[Cl;D1;H0:13]):[c:11]:[c:12].[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5].[ClH;D0;+0:10]
null
[]
null
null
5
HOUR
4N Hydrochloric acid/ethyl acetate solution (20 mL) and ethanol (10 mL) were added to tert-butyl 4-{4-[(5-{2-[2-(benzoyloxy)ethoxy]ethyl}-5H-pyrrolo[3,2-d]pyrimidin-4-yl)amino]-2-chlorophenoxy}piperidine-1-carboxylate (3.82 g), and the mixture was stirred at room temperature for 5 hrs. The reaction mixture was concentr...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ether.Boc
Aromatic halide.Secondary amine
C1CC[NH]CC1.c1ccccc1
c1ccccc1.C1CCNCC1
c1ncnc2cc[nH]c12.c1ccccc1.C1CCNCC1.c1ccccc1
HO-
C(C)O
null
5
CC(C)(C)OC(=O)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)CC1>C(C)O>Cl.O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b5f1f56301ff4b608fed21fa38c80fa3
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1.O=C=Nc1c(F)cccc1F>>O=C(Nc1c(F)cccc1F)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
FC1=C(C(=CC=C1)F)N=C=O.Cl.Cl.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2CCNCC2)Cl.C([O-])([O-])=O.[Na+].[Na+].C(C)(=O)OCC>>Cl.ClC1=C(OC2CCN(CC2)C(=O)NC2=C(C=CC=C2F)F)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO
O=C(c1ccccc1)[O:36][CH2:35][CH2:34][O:33][CH2:32][CH2:31][n:30]1[cH:29][cH:28][c:27]2[n:26][cH:25][n:24][c:23]([NH:22][c:21]3[cH:20][cH:19][c:18]([O:17][CH:16]4[CH2:15][CH2:14][NH:13][CH2:42][CH2:41]4)[c:39]([Cl:40])[cH:38]3)[c:37]21.[O:2]=[C:3]=[N:4][c:5]1[c:6]([F:7])[cH:8][cH:9][cH:10][c:11]1[F:12]>>[O:2]=[C:3]([NH:4...
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1.O=C=Nc1c(F)cccc1F
O=C(Nc1c(F)cccc1F)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
null
null
O1CCCC1.O
Acylation
OtherReaction
3d5daa558c514eafe4a8e588e22c05699c195e8e75bc26b521cf6a1e2dce1526
06668a26d5e7eeaa79479805e8a93d257d5e64cf3a8d52ffd96b865a7e33864c
O=C(Nc1ccccc1)N1CCC(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)CC1
O=C(-[O;H0;D2;+0:1]-[C:2]-[C:3])-c1:c:c:c:c:c:1.[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8].[O;D1;H0:9]=[C;H0;D2;+0:10]=[N;H0;D2;+0:11]-[c:12](:[c:13]):[c:14]>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[C;H0;D3;+0:10](=[O;D1;H0:9])-[NH;D2;+0:11]-[c:12](:[c:13]):[c:14])-[C:7]-[C:8].[C:3]-[C:2]-[OH;D1;+0:1]
129.4
[{"value": 129.4, "product": "Cl.ClC1=C(OC2CCN(CC2)C(=O)NC2=C(C=CC=C2F)F)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a mixture of 2-[2-(4-{[3-chloro-4-(piperidin-4-yloxy)phenyl]amino}-5H-pyrrolo[3,2-d]pyrimidin-5-yl)ethoxy]ethyl benzoate dihydrochloride (305 mg), 10% aqueous sodium carbonate solution (10 mL), ethyl acetate (15 mL) and tetrahydrofuran (5 mL) was added 2,6-difluorophenyl isocyanate (93 mg) with vigorous stirring. Th...
10.6084/m9.figshare.5104873.v1
null
Ester.Isocyanate.Secondary amine
Urea.Primary alcohol
c1ccccc1.C1CCNCC1
C1CC[NH]CC1
c1ccccc1.C1CC[NH]CC1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O1CCCC1.O
null
2
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1.O=C=Nc1c(F)cccc1F>O1CCCC1.O>O=C(Nc1c(F)cccc1F)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c8d45ef7341e4a259527df19d4d59b92
NC1CCCC1.O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1.O=C(n1ccnc1)n1ccnc1>>O=C(NC1CCCC1)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
C(=O)(N1C=NC=C1)N1C=NC=C1.C1(CCCC1)N.Cl.Cl.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2CCNCC2)Cl.C(C)N(CC)CC>>Cl.ClC1=C(OC2CCN(CC2)C(=O)NC2CCCC2)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO
[NH2:4][CH:5]1[CH2:6][CH2:7][CH2:8][CH2:9]1.O=C(c1ccccc1)[O:33][CH2:32][CH2:31][O:30][CH2:29][CH2:28][n:27]1[cH:26][cH:25][c:24]2[n:23][cH:22][n:21][c:20]([NH:19][c:18]3[cH:17][cH:16][c:15]([O:14][CH:13]4[CH2:12][CH2:11][NH:10][CH2:39][CH2:38]4)[c:36]([Cl:37])[cH:35]3)[c:34]21.c1cn([C:3](n2ccnc2)=[O:2])cn1>>[O:2]=[C:3]...
NC1CCCC1.O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1.O=C(n1ccnc1)n1ccnc1
O=C(NC1CCCC1)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
null
null
O1CCCC1.O
Acylation
OtherReaction
22d4a029fb0269f180201dea5604d2f55ee37dab9d1efc34f915507d4c3359e6
14aff967099df1655de24622d6738511aed25e5de6dfcd9146c67d3e73427243
O=C(NC1CCCC1)N1CCC(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)CC1
O=C(-[O;H0;D2;+0:1]-[C:2]-[C:3])-c1:c:c:c:c:c:1.[C:4]-[C:5]-[NH;D2;+0:6]-[C:7]-[C:8].[C:9]-[C:10](-[NH2;D1;+0:11])-[C:12].[O;D1;H0:13]=[C;H0;D3;+0:14](-n1:c:c:n:c:1)-n1:c:c:n:c:1>>[C:4]-[C:5]-[N;H0;D3;+0:6](-[C;H0;D3;+0:14](=[O;D1;H0:13])-[NH;D2;+0:11]-[C:10](-[C:9])-[C:12])-[C:7]-[C:8].[C:3]-[C:2]-[OH;D1;+0:1]
129.5
[{"value": 129.5, "product": "Cl.ClC1=C(OC2CCN(CC2)C(=O)NC2CCCC2)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 1,1′-carbonylbis(1H-imidazole) (162 mg) in tetrahydrofuran (5 mL) was added a solution of cyclopentylamine (85 mg) in tetrahydrofuran (1 mL), and the mixture was stirred at room temperature for 1 hr. A solution of 2-[2-(4-{[3-chloro-4-(piperidin-4-yloxy)phenyl]amino}-5H-pyrrolo[3,2-d]pyrimidin-5-yl)eth...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine.Secondary amine
Urea.Primary alcohol
c1ccccc1.C1CCNCC1.c1c[nH]cn1.c1c[nH]cn1
C1CC[NH]CC1
C1CCCC1.C1CC[NH]CC1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O1CCCC1.O
null
1
NC1CCCC1.O=C(OCCOCCn1ccc2ncnc(Nc3ccc(OC4CCNCC4)c(Cl)c3)c21)c1ccccc1.O=C(n1ccnc1)n1ccnc1>O1CCCC1.O>O=C(NC1CCCC1)N1CCC(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)CC1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-1d8295f4118c443f845dfe6d506868df
CC(C)(C)OC(=O)c1ccc(Oc2ccc(N)cc2Cl)cc1.O=C(OCCOCCn1ccc2ncnc(Cl)c21)c1ccccc1>>CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)Cl.NC1=CC(=C(OC2=CC=C(C(=O)OC(C)(C)C)C=C2)C=C1)Cl>>C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)OC(C)(C)C)C=C1)C=C2)Cl
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([O:12][c:13]2[cH:14][cH:15][c:16]([NH2:17])[cH:41][c:42]2[Cl:43])[cH:44][cH:45]1.Cl[c:18]1[n:19][cH:20][n:21][c:22]2[cH:23][cH:24][n:25]([CH2:26][CH2:27][O:28][CH2:29][CH2:30][O:31][C:32](=[O:33])[c:34]3[cH:35][cH:36][cH:37][cH:38][cH:39]3)[c:40]...
CC(C)(C)OC(=O)c1ccc(Oc2ccc(N)cc2Cl)cc1.O=C(OCCOCCn1ccc2ncnc(Cl)c21)c1ccccc1
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
null
null
C(C)(C)O
Heteroatom Alkylation and Arylation
Goldberg coupling aryl amine-aryl chloride
b3e82b6ead9cdf4e2f8cbbcf91109747f4dd1119eb8fb5a3a7a9710387d7d6e5
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(Oc4ccccc4)cc3)c21)c1ccccc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[#7;a:4]:[c:5]2:[c:6]:[c:7]:[#7;a:8](-[C:9]):[c:10]:2:1.[NH2;D1;+0:11]-[c:12](:[c:13]):[c:14]>>[C:9]-[#7;a:8]1:[c:7]:[c:6]:[c:5]2:[#7;a:4]:[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:11]-[c:12](:[c:13]):[c:14]):[c:10]:1:2
58
[{"value": 58.0, "product": "C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)OC(C)(C)C)C=C1)C=C2)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
80
CELSIUS
8
HOUR
A mixture of 2-[2-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-5-yl)ethoxy]ethyl benzoate (1.46 g), tert-butyl 4-(4-amino-2-chlorophenoxy)benzoate (1.35 g) and isopropyl alcohol (30 mL) was stirred at 80° C. overnight. The reaction mixture was concentrated under reduced pressure, water and saturated aqueous sodium hydrogen car...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ncnc2cc[nH]c12
c1ncnc2cc[nH]c12
c1ccccc1.c1ccccc1.c1ncnc2cc[nH]c12.c1ccccc1
HCl
C(C)(C)O
80
8
CC(C)(C)OC(=O)c1ccc(Oc2ccc(N)cc2Cl)cc1.O=C(OCCOCCn1ccc2ncnc(Cl)c21)c1ccccc1>C(C)(C)O>CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fb3ce3baa25c49f88b01937ad41ccc0d
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1>>CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)cc1.Cl
C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)OC(C)(C)C)C=C1)C=C2)Cl.O>>Cl.ClC1=C(OC2=CC=C(C(=O)OC(C)(C)C)C=C2)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO
O=C(c1ccccc1)[O:31][CH2:30][CH2:29][O:28][CH2:27][CH2:26][n:25]1[cH:24][cH:23][c:22]2[n:21][cH:20][n:19][c:18]([NH:17][c:16]3[cH:15][cH:14][c:13]([O:12][c:11]4[cH:10][cH:9][c:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[cH:37][cH:36]4)[c:34]([Cl:35])[cH:33]3)[c:32]21>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[...
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)cc1.Cl
null
null
O1CCCC1.CO.[OH-].[Na+]
Miscellaneous
Hydrolysis or Hydrogenolysis of Carboxylic Esters or Thioesters
75c7457e3a9fb6f1ba09eb81042cf77dcdbcc742bd16c83aaeebe9a9679aff92
6c68e56451f63eb914da47d835c80c50f16b8e098a52b924c7914bb1a69fa96c
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
O=C(-[O;H0;D2;+0:1]-[C:2]-[C:3])-c1:c:c:c:c:c:1>>[C:3]-[C:2]-[OH;D1;+0:1]
193.3
[{"value": 193.3, "product": "Cl.ClC1=C(OC2=CC=C(C(=O)OC(C)(C)C)C=C2)C=CC(=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
tert-Butyl 4-{4-[(5-{2-[2-(benzoyloxy)ethoxy]ethyl}-5H-pyrrolo[3,2-d]pyrimidin-4-yl)amino]-2-chlorophenoxy}benzoate (189 mg) was dissolved in a mixed solvent of methanol (5 mL) and tetrahydrofuran (1 mL), 1N aqueous sodium hydroxide solution (0.6 mL) was added, and the mixture was stirred overnight at room temperature....
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
c1ccccc1
null
c1ccccc1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O1CCCC1.CO.[OH-].[Na+]
null
8
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1>O1CCCC1.CO.[OH-].[Na+]>CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)cc1.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ea89cb9c33614f4182b2a959ee003cb3
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1>>Cl.O=C(O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)OC(C)(C)C)C=C1)C=C2)Cl>>Cl.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)O)C=C1)C=C2)Cl
CC(C)(C)[O:4][C:3](=[O:2])[c:5]1[cH:6][cH:7][c:8]([O:9][c:10]2[cH:11][cH:12][c:13]([NH:14][c:15]3[n:16][cH:17][n:18][c:19]4[cH:20][cH:21][n:22]([CH2:23][CH2:24][O:25][CH2:26][CH2:27][O:28][C:29](=[O:30])[c:31]5[cH:32][cH:33][cH:34][cH:35][cH:36]5)[c:37]34)[cH:38][c:39]2[Cl:1])[cH:41][cH:42]1>>[ClH:1].[O:2]=[C:3]([OH:4]...
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
Cl.O=C(O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
null
null
FC(C(=O)O)(F)F
Functional Group Interconversion
Deprotection of carboxylic acid
2925f84c790135189a05fa87f9d873359f8ae83f30057d47d934c52331b0a572
882ec6822f5a850b1be02ee0d833b619e124b3402656234509adb466b745d330
O=C(OCCOCCn1ccc2ncnc(Nc3ccc(Oc4ccccc4)cc3)c21)c1ccccc1
C-C(-C)(-C)-[O;H0;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[#8:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[Cl;H0;D1;+0:9]):[c:10]:[c:11]>>[#8:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[Cl;D1;H0:12]):[c:10]:[c:11].[O;D1;H0:3]=[C:2](-[OH;D1;+0:1])-[c:4].[ClH;D0;+0:9]
190.1
[{"value": 190.1, "product": "Cl.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)O)C=C1)C=C2)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Trifluoroacetic acid (10 mL) was added to tert-butyl 4-{4-[(5-{2-[2-(benzoyloxy)ethoxy]ethyl}-5H-pyrrolo[3,2-d]pyrimidin-4-yl)amino]-2-chlorophenoxy}benzoate (1.26 g), and the mixture was stirred at room temperature for 3 hrs. The reaction mixture was concentrated under reduced pressure, 4N hydrochloric acid/ethyl acet...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ester.Boc
Aromatic halide.Carboxylic acid
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1.c1ncnc2cc[nH]c12.c1ccccc1
Other
FC(C(=O)O)(F)F
null
3
CC(C)(C)OC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1>FC(C(=O)O)(F)F>Cl.O=C(O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e05cd2b1739249729b201ad1248b5921
CC(C)(C)N.O=C(O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1>>CC(C)(C)NC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)cc1
Cl.C(C1=CC=CC=C1)(=O)OCCOCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(OC1=CC=C(C(=O)O)C=C1)C=C2)Cl.CC(C)(C)N.Cl.C(C)N=C=NCCCN(C)C.O.ON1N=NC2=C1C=CC=C2>>Cl.C(C)(C)(C)NC(C1=CC=C(C=C1)OC1=C(C=C(C=C1)NC=1C2=C(N=CN1)C=CN2CCOCCO)Cl)=O
[CH3:1][C:2]([CH3:3])([CH3:4])[NH2:5].O=C(c1ccccc1)[O:31][CH2:30][CH2:29][O:28][CH2:27][CH2:26][n:25]1[cH:24][cH:23][c:22]2[n:21][cH:20][n:19][c:18]([NH:17][c:16]3[cH:15][cH:14][c:13]([O:12][c:11]4[cH:10][cH:9][c:8]([C:6](O)=[O:7])[cH:37][cH:36]4)[c:34]([Cl:35])[cH:33]3)[c:32]21>>[CH3:1][C:2]([CH3:3])([CH3:4])[NH:5][C:...
CC(C)(C)N.O=C(O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1
CC(C)(C)NC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)cc1
null
null
O.C(C)N(CC)CC.CN(C=O)C
Acylation
OtherReaction
841820a51f305a54d171f5504c9b8e43f1508e4bf73cd8b690ba0db9886e7c72
5f68606e1652dcb7d724fc9313be32cd73fe12aa10c1a7ff593e99a300f09c8e
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].O=C(-[O;H0;D2;+0:6]-[C:7]-[C:8])-c1:c:c:c:c:c:1.[C;D1;H3:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[NH2;D1;+0:13]>>[C;D1;H3:9]-[C:10](-[C;D1;H3:11])(-[C;D1;H3:12])-[NH;D2;+0:13]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:8]-[C:7]-[OH;D1;+0:6]
null
[]
null
null
8
HOUR
A mixture of 4-{4-[(5-{2-[2-(benzoyloxy)ethoxy]ethyl}-5H-pyrrolo[3,2-d]pyrimidin-4-yl)amino]-2-chlorophenoxy}benzoic acid hydrochloride (183 mg), 2-methylpropan-2-amine (0.038 mL), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (69 mg), 1-hydroxybenzotriazole monohydrate (55 mg), triethylamine (0.050 mL) a...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ester.Primary amine
Secondary amide.Primary alcohol
c1ccccc1
null
c1ccccc1.c1ccccc1.c1ncnc2cc[nH]c12
HO-
O.C(C)N(CC)CC.CN(C=O)C
null
8
CC(C)(C)N.O=C(O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCOC(=O)c5ccccc5)c34)cc2Cl)cc1>O.C(C)N(CC)CC.CN(C=O)C>CC(C)(C)NC(=O)c1ccc(Oc2ccc(Nc3ncnc4ccn(CCOCCO)c34)cc2Cl)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-69a6a307d91545ee921a24863af1aeca
CN(C(=O)OC(C)(C)C)C(=NC(=O)OC(C)(C)C)n1cccn1.Cl.NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>>CNC(=N)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21.Cl
O.CN(C(=NC(=O)OC(C)(C)C)N1N=CC=C1)C(=O)OC(C)(C)C.C(C)N(C(C)C)C(C)C.Cl.Cl.NCCN1C=CC=2N=CN=C(C21)NC2=CC(=C(C=C2)OC2=CC(=CC=C2)C(F)(F)F)Cl>>Cl.Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(=N)NC
CC(C)(C)OC(=O)[N:2]([CH3:1])[C:3](n1cccn1)=[N:4]C(=O)OC(C)(C)C.[ClH:37].[NH2:5][CH2:6][CH2:7][n:8]1[cH:9][cH:10][c:11]2[n:12][cH:13][n:14][c:15]([NH:16][c:17]3[cH:18][cH:19][c:20]([O:21][c:22]4[cH:23][cH:24][cH:25][c:26]([C:27]([F:28])([F:29])[F:30])[cH:31]4)[c:32]([Cl:33])[cH:34]3)[c:35]12>>[CH3:1][NH:2][C:3](=[NH:4])...
CN(C(=O)OC(C)(C)C)C(=NC(=O)OC(C)(C)C)n1cccn1.Cl.NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21
CNC(=N)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21.Cl
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
74ac281d7376101e04892b698126e6c95ded993b43965c546e5a0d6545da3e9b
a03ac3c151f67cf6329b1139a3d31f02d5af7d1dceec1cac28a151c281788780
c1ccc(Oc2ccc(Nc3ncnc4cc[nH]c34)cc2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D2;+0:1]=[C;H0;D3;+0:2](-[N;H0;D3;+0:3](-[C;D1;H3:4])-C(=O)-O-C(-C)(-C)-C)-n1:c:c:c:n:1.[C:5]-[C:6]-[NH2;D1;+0:7]>>[C:5]-[C:6]-[NH;D2;+0:7]-[C;H0;D3;+0:2](=[NH;D1;+0:1])-[NH;D2;+0:3]-[C;D1;H3:4]
88.5
[{"value": 88.5, "product": "Cl.Cl.ClC=1C=C(C=CC1OC1=CC(=CC=C1)C(F)(F)F)NC=1C2=C(N=CN1)C=CN2CCNC(=N)NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
DAY
To a solution of N-methyl-N,N′-bis(tert-butoxy carbonyl)-1H-pyrazole-1-carboxamidine (138 mg) and ethyldiisopropylamine (0.16 mL) in acetonitrile (4 mL) was added 5-(2-aminoethyl)-N-{3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}-5H-pyrrolo[3,2-d]pyrimidin-4-amine dihydrochloride (200 mg), and the mixture was stirred a...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Ether.Primary amine.Boc.Boc
Secondary amine.Secondary amine
c1cn[nH]c1
null
c1ncnc2cc[nH]c12.c1ccccc1.c1ccccc1
HO-
C(C)#N
null
96
CN(C(=O)OC(C)(C)C)C(=NC(=O)OC(C)(C)C)n1cccn1.Cl.NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21>C(C)#N>CNC(=N)NCCn1ccc2ncnc(Nc3ccc(Oc4cccc(C(F)(F)F)c4)c(Cl)c3)c21.Cl
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d36e84f0fd644ef7b9900b0fd0ff2d69
O=[N+]([O-])c1ccc(F)c(Cl)c1.Oc1ccc(CCCn2ccnc2)cc1>>O=[N+]([O-])c1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
O.N1(C=NC=C1)CCCC1=CC=C(C=C1)O.ClC=1C=C(C=CC1F)[N+](=O)[O-].C([O-])([O-])=O.[K+].[K+]>>ClC=1C=C(C=CC1OC1=CC=C(C=C1)CCCN1C=NC=C1)[N+](=O)[O-]
F[c:7]1[cH:6][cH:5][c:4]([N+:2](=[O:1])[O-:3])[cH:25][c:23]1[Cl:24].[OH:8][c:9]1[cH:10][cH:11][c:12]([CH2:13][CH2:14][CH2:15][n:16]2[cH:17][cH:18][n:19][cH:20]2)[cH:21][cH:22]1>>[O:1]=[N+:2]([O-:3])[c:4]1[cH:5][cH:6][c:7]([O:8][c:9]2[cH:10][cH:11][c:12]([CH2:13][CH2:14][CH2:15][n:16]3[cH:17][cH:18][n:19][cH:20]3)[cH:21...
O=[N+]([O-])c1ccc(F)c(Cl)c1.Oc1ccc(CCCn2ccnc2)cc1
O=[N+]([O-])c1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
null
null
CN(C=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
e4ea1e38252bc3b9c5ec04486386725e6570ab3860d45e337a1d131319bbf0fc
27e9a6bab4e3ed54aeb6be4d84cb1c0170208288795e252a46e57e44ecc064f0
c1ccc(Oc2ccc(CCCn3ccnc3)cc2)cc1
F-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[Cl;D1;H0:5]):[c:6].[OH;D1;+0:7]-[c:8](:[c:9]):[c:10]>>[Cl;D1;H0:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[O;H0;D2;+0:7]-[c:8](:[c:9]):[c:10]):[c:2]:[c:3]
93.4
[{"value": 93.4, "product": "ClC=1C=C(C=CC1OC1=CC=C(C=C1)CCCN1C=NC=C1)[N+](=O)[O-]", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of 4-[3-(1H-imidazol-1-yl)propyl]phenol (405 mg) and 3-chloro-4-fluoronitrobenzene (370 mg) in N,N-dimethylformamide (4 mL) was added potassium carbonate (415 mg), and the mixture was stirred at room temperature for 16 hrs. Under ice-cooling, water was added and the mixture was extracted with ethyl acetat...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aromatic alcohol
Ether
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1.c1c[nH]cn1
HF
CN(C=O)C
null
16
O=[N+]([O-])c1ccc(F)c(Cl)c1.Oc1ccc(CCCn2ccnc2)cc1>CN(C=O)C>O=[N+]([O-])c1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9f3ea9e203b14268bbef232e96c7413e
O=[N+]([O-])c1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1>>Nc1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
ClC=1C=C(C=CC1OC1=CC=C(C=C1)CCCN1C=NC=C1)[N+](=O)[O-]>>ClC=1C=C(N)C=CC1OC1=CC=C(C=C1)CCCN1C=NC=C1
O=[N+:1]([O-])[c:2]1[cH:3][cH:4][c:5]([O:6][c:7]2[cH:8][cH:9][c:10]([CH2:11][CH2:12][CH2:13][n:14]3[cH:15][cH:16][n:17][cH:18]3)[cH:19][cH:20]2)[c:21]([Cl:22])[cH:23]1>>[NH2:1][c:2]1[cH:3][cH:4][c:5]([O:6][c:7]2[cH:8][cH:9][c:10]([CH2:11][CH2:12][CH2:13][n:14]3[cH:15][cH:16][n:17][cH:18]3)[cH:19][cH:20]2)[c:21]([Cl:22]...
O=[N+]([O-])c1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
Nc1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
null
[Pt]
CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
c1ccc(Oc2ccc(CCCn3ccnc3)cc2)cc1
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
45.2
[{"value": 45.2, "product": "ClC=1C=C(N)C=CC1OC1=CC=C(C=C1)CCCN1C=NC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
16
HOUR
To a solution of 3-chloro-4-{4-[3-(1H-imidazol-1-yl)propyl]phenoxy}nitrobenzene (669 mg) in methanol (7 mL) was added 5% Pt/C (140 mg), and the mixture was stirred under hydrogen atmosphere at room temperature for 16 hrs. 5% Pt/C was filtered off and the filtrate was concentrated. The residue was purified by basic sili...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccccc1.c1ccccc1.c1c[nH]cn1
Other
[Pt].CO
null
16
O=[N+]([O-])c1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1>[Pt].CO>Nc1ccc(Oc2ccc(CCCn3ccnc3)cc2)c(Cl)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-89b849bfcf45431dbc41fad8bbb3c08c
CC(C)c1ccc(C=O)cc1.[OH-]>>CC(C)c1ccc(C(O)C(=O)O)cc1
[Cl-].[Li+].[OH-].[K+].Cl.C(Br)(Br)Br.C(C)(C)C1=CC=C(C=O)C=C1.O1CCOCC1>>OC(C(=O)O)C1=CC=C(C=C1)C(C)C
[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH:8]=[O:9])[cH:13][cH:14]1.[OH-:12]>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH:8]([OH:9])[C:10](=[O:11])[OH:12])[cH:13][cH:14]1
CC(C)c1ccc(C=O)cc1.[OH-]
CC(C)c1ccc(C(O)C(=O)O)cc1
null
null
null
Acylation
OtherReaction
e4754e3793ba0362af7cd262e2f320471fced6da69cfa59aaf69349f987b0106
7b79ddb9582ae558ef0424125dcd16c236a764b78e4d8d3057436676b03c02cd
c1ccccc1
[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5].[OH-;D0:6]>>[O;D1;H0:7]=[C:8](-[OH;D1;+0:6])-[CH;D3;+0:2](-[OH;D1;+0:1])-[c:3](:[c:4]):[c:5]
73
[{"value": 73.0, "product": "OC(C(=O)O)C1=CC=C(C=C1)C(C)C", "details": "PERCENTYIELD", "is_desired": false}]
7.5
CELSIUS
24
HOUR
To a mixture of lithium chloride (17.0 g, 418 mmol), potassium hydroxide (44.9 g, 800 mmol) and ice (150 g) was added a solution of bromoform (17.5 mL, 200 mmol) and 4-isopropyl benzaldehyde (30.3 mL, 200 mmol) in 1,4-dioxane (150 mL) at 0° C., and the mixture was stirred at 5-10° C. for 24 hours and then stirred at 35...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Carboxylic acid.Secondary alcohol
null
null
c1ccccc1
null
null
7.5
24
CC(C)c1ccc(C=O)cc1.[OH-]>>CC(C)c1ccc(C(O)C(=O)O)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-4bc535bc95c94d88b2c7233959430bd8
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cc(C)c(C)c(O)c1>>Cc1cc(C)c2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
S(O)(O)(=O)=O.OC(C(=O)O)C1=CC=C(C=C1)C(C)C.CC1=C(C=C(C=C1C)C)O>>C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C(=CC(=C2C)C)C)=O
O[CH:13]([C:11]([OH:10])=[O:12])[c:14]1[cH:15][cH:16][c:17]([CH:18]([CH3:19])[CH3:20])[cH:21][cH:22]1.O[c:7]1[cH:6][c:4]([CH3:5])[cH:3][c:2]([CH3:1])[c:8]1[CH3:9]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:7]([c:8]1[CH3:9])[O:10][C:11](=[O:12])[CH:13]2[c:14]1[cH:15][cH:16][c:17]([CH:18]([CH3:19])[CH3:20])[cH:21][cH:22]...
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cc(C)c(C)c(O)c1
Cc1cc(C)c2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
a36a17d3b5a98a14927a5ab2b0be42d209b866ef66a0bb2bbf9dcb43cad4f8d7
908e0f9e50a05a6374ff137c29a63b494c9fdcd7afae396ae828385ea73c4999
O=C1Oc2ccccc2C1c1ccccc1
O-[CH;D3;+0:1](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4])-[c:5](:[c:6]):[c:7].O-[c;H0;D3;+0:8]1:[cH;D2;+0:9]:[c:10](-[C;D1;H3:11]):[c:12]:[c:13]:[c:14]:1-[C;D1;H3:15]>>[C;D1;H3:11]-[c:10]1:[c:12]:[c:13]:[c:14](-[C;D1;H3:15]):[c;H0;D3;+0:8]2:[c;H0;D3;+0:9]:1-[CH;D3;+0:1](-[c:5](:[c:6]):[c:7])-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-...
65
[{"value": 65.0, "product": "C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C(=CC(=C2C)C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
115
CELSIUS
12
HOUR
To a mixture of hydroxy(4-isopropylphenyl)acetic acid synthesized in Reference Example 1 (11.8 g, 60.8 mmol) and 2,3,5-trimethylphenol (12.4 g, 91.2 mmol) was added 70% sulfuric acid (10 mL) at room temperature, and the mixture was stirred at 115° C. for 12 hours. The mixture was added to water and was extracted with d...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol.Aromatic alcohol
Ester
c1ccccc1
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
O
115
12
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cc(C)c(C)c(O)c1>O>Cc1cc(C)c2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fc955fdcc913432a83d75d1cbc759b22
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cccc(O)c1C>>Cc1ccc2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
OC(C(=O)O)C1=CC=C(C=C1)C(C)C.CC1=C(C=CC=C1C)O>>C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C=CC(=C2C)C)=O
O[C:10](=[O:11])[CH:12](O)[c:13]1[cH:14][cH:15][c:16]([CH:17]([CH3:18])[CH3:19])[cH:20][cH:21]1.[CH3:1][c:2]1[cH:3][cH:4][cH:5][c:6]([OH:9])[c:7]1[CH3:8]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([c:7]1[CH3:8])[O:9][C:10](=[O:11])[CH:12]2[c:13]1[cH:14][cH:15][c:16]([CH:17]([CH3:18])[CH3:19])[cH:20][cH:21]1
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cccc(O)c1C
Cc1ccc2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
null
null
CO
Acylation
OtherReaction
a9a5b73428c6cee8742382adf23f6cccf5c4cf75079871710fa49d52d876205d
7c7c21ef6846a89a0c7e34038d2f8c5934b71c90169d827b6b3d7f9d687374a5
O=C1Oc2ccccc2C1c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH;D3;+0:3](-O)-[c:4](:[c:5]):[c:6].[OH;D1;+0:7]-[c:8](:[c:9]):[cH;D2;+0:10]:[c:11]:[c:12]>>[O;D1;H0:2]=[C;H0;D3;+0:1]1-[O;H0;D2;+0:7]-[c:8](:[c:9]):[c;H0;D3;+0:10](:[c:11]:[c:12])-[CH;D3;+0:3]-1-[c:4](:[c:5]):[c:6]
44
[{"value": 44.0, "product": "C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C=CC(=C2C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using hydroxy(4-isopropylphenyl)acetic acid synthesized in Reference Example 1 and 2,3-dimethylphenol, the title compound was synthesized in the same manner as in Reference Example 2. Yield 44%. Melting point: 58-60° C. (methanol). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol.Aromatic alcohol
Ester
c1ccccc1
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
CO
null
null
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cccc(O)c1C>CO>Cc1ccc2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-2ac38c1facb84f86b9199d8773e793b9
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cc(C)cc(O)c1>>Cc1cc(C)c2c(c1)OC(=O)C2c1ccc(C(C)C)cc1
OC(C(=O)O)C1=CC=C(C=C1)C(C)C.CC=1C=C(C=C(C1)C)O>>C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C(=CC(=C2)C)C)=O
O[CH:12]([C:10]([OH:9])=[O:11])[c:13]1[cH:14][cH:15][c:16]([CH:17]([CH3:18])[CH3:19])[cH:20][cH:21]1.O[c:7]1[cH:6][c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:8]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:7]([cH:8]1)[O:9][C:10](=[O:11])[CH:12]2[c:13]1[cH:14][cH:15][c:16]([CH:17]([CH3:18])[CH3:19])[cH:20][cH:21]1
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cc(C)cc(O)c1
Cc1cc(C)c2c(c1)OC(=O)C2c1ccc(C(C)C)cc1
null
null
C(C)(=O)OCC.CCCCCC
Heteroatom Alkylation and Arylation
OtherReaction
a36a17d3b5a98a14927a5ab2b0be42d209b866ef66a0bb2bbf9dcb43cad4f8d7
908e0f9e50a05a6374ff137c29a63b494c9fdcd7afae396ae828385ea73c4999
O=C1Oc2ccccc2C1c1ccccc1
O-[CH;D3;+0:1](-[C:2](=[O;D1;H0:3])-[OH;D1;+0:4])-[c:5](:[c:6]):[c:7].O-[c;H0;D3;+0:8]1:[c:9]:[c:10]:[c:11]:[c:12](-[C;D1;H3:13]):[cH;D2;+0:14]:1>>[C;D1;H3:13]-[c:12]1:[c:11]:[c:10]:[c:9]:[c;H0;D3;+0:8]2:[c;H0;D3;+0:14]:1-[CH;D3;+0:1](-[c:5](:[c:6]):[c:7])-[C:2](=[O;D1;H0:3])-[O;H0;D2;+0:4]-2
45
[{"value": 45.0, "product": "C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C(=CC(=C2)C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using hydroxy(4-isopropylphenyl)acetic acid synthesized in Reference Example 1 and 3,5-dimethylphenol, the title compound was synthesized in the same manner as in Reference Example 2. Yield 45%. Melting point: 76-77° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol.Aromatic alcohol
Ester
c1ccccc1
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
C(C)(=O)OCC.CCCCCC
null
null
CC(C)c1ccc(C(O)C(=O)O)cc1.Cc1cc(C)cc(O)c1>C(C)(=O)OCC.CCCCCC>Cc1cc(C)c2c(c1)OC(=O)C2c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c742566f1151421f8fc9dceb5b8cab0d
CC(C)c1ccc(C(O)C(=O)O)cc1.Oc1ccc(Br)cc1>>CC(C)c1ccc(C2C(=O)Oc3ccc(Br)cc32)cc1
OC(C(=O)O)C1=CC=C(C=C1)C(C)C.BrC1=CC=C(C=C1)O>>BrC=1C=CC2=C(C(C(O2)=O)C2=CC=C(C=C2)C(C)C)C1
O[CH:8]([c:7]1[cH:6][cH:5][c:4]([CH:2]([CH3:1])[CH3:3])[cH:20][cH:19]1)[C:9](O)=[O:10].[OH:11][c:12]1[cH:13][cH:14][c:15]([Br:16])[cH:17][cH:18]1>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH:8]2[C:9](=[O:10])[O:11][c:12]3[cH:13][cH:14][c:15]([Br:16])[cH:17][c:18]32)[cH:19][cH:20]1
CC(C)c1ccc(C(O)C(=O)O)cc1.Oc1ccc(Br)cc1
CC(C)c1ccc(C2C(=O)Oc3ccc(Br)cc32)cc1
null
null
CO
Acylation
OtherReaction
a9a5b73428c6cee8742382adf23f6cccf5c4cf75079871710fa49d52d876205d
7c7c21ef6846a89a0c7e34038d2f8c5934b71c90169d827b6b3d7f9d687374a5
O=C1Oc2ccccc2C1c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH;D3;+0:3](-O)-[c:4](:[c:5]):[c:6].[OH;D1;+0:7]-[c:8](:[c:9]):[cH;D2;+0:10]:[c:11]:[c:12]>>[O;D1;H0:2]=[C;H0;D3;+0:1]1-[O;H0;D2;+0:7]-[c:8](:[c:9]):[c;H0;D3;+0:10](:[c:11]:[c:12])-[CH;D3;+0:3]-1-[c:4](:[c:5]):[c:6]
30
[{"value": 30.0, "product": "BrC=1C=CC2=C(C(C(O2)=O)C2=CC=C(C=C2)C(C)C)C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using hydroxy(4-isopropylphenyl)acetic acid synthesized in Reference Example 1 and 4-bromophenol, the title compound was synthesized in the same manner as in Reference Example 2. Yield 30%. Melting point: 157-158° C. (methanol). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Secondary alcohol.Aromatic alcohol
Ester
c1ccccc1
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
HO-
CO
null
null
CC(C)c1ccc(C(O)C(=O)O)cc1.Oc1ccc(Br)cc1>CO>CC(C)c1ccc(C2C(=O)Oc3ccc(Br)cc32)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-6bdb09d3125a4f06bb2a77dcbd47cfc5
CI.Cc1cc(C)c2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1>>Cc1cc(C)c2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1
C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C(=CC(=C2C)C)C)=O.CI.[H-].[Na+].O>>C(C)(C)C1=CC=C(C=C1)C1(C(OC2=C1C(=CC(=C2C)C)C)=O)C
I[CH3:14].[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:7]([c:8]1[CH3:9])[O:10][C:11](=[O:12])[CH:13]2[c:15]1[cH:16][cH:17][c:18]([CH:19]([CH3:20])[CH3:21])[cH:22][cH:23]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:7]([c:8]1[CH3:9])[O:10][C:11](=[O:12])[C:13]2([CH3:14])[c:15]1[cH:16][cH:17][c:18]([CH:19]([CH3:20])[CH3:21])...
CI.Cc1cc(C)c2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1
Cc1cc(C)c2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1
null
null
CN(C)C=O
C-C Coupling
Methylation with MeI_tertiary
2df58dbc7598f4dd7d1f88d398506f8000fc8f56173da0fda4f1729c49cd7825
49d6f28766066d07dffbcc6f4da77792f6ba67b4de619800bad651525d6fe2e7
O=C1Oc2ccccc2C1c1ccccc1
I-[CH3;D1;+0:1].[O;D1;H0:2]=[C:3]1-[#8:4]-[c:5]:[c:6](:[c:7])-[CH;D3;+0:8]-1-[c:9](:[c:10]):[c:11]>>[CH3;D1;+0:1]-[C;H0;D4;+0:8]1(-[c:9](:[c:10]):[c:11])-[C:3](=[O;D1;H0:2])-[#8:4]-[c:5]:[c:6]-1:[c:7]
94
[{"value": 94.0, "product": "C(C)(C)C1=CC=C(C=C1)C1(C(OC2=C1C(=CC(=C2C)C)C)=O)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 3-(4-isopropylphenyl)-4,6,7-trimethyl-1-benzofuran-2(3H)-one synthesized in Reference Example 2 (2.10 g, 7.13 mmol) in DMF (30 mL) was added sodium hydride (a 60% fluidized paraffin dispersion, 314 mg, 7.84 mmol) at 0° C., and the mixture was stirred at room temperature for 30 minutes. To the reaction ...
10.6084/m9.figshare.5104873.v1
null
Ester
Ester
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HI
CN(C)C=O
null
0.5
CI.Cc1cc(C)c2c(c1C)OC(=O)C2c1ccc(C(C)C)cc1>CN(C)C=O>Cc1cc(C)c2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-38992cda04e74b71804393b32ed6a00d
Cc1cc(C)c2c(c1)OC(=O)C2c1ccc(C(C)C)cc1>>Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1
C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C(=CC(=C2)C)C)=O>>OCC(C1=CC=C(C=C1)C(C)C)C1=C(C=C(C=C1C)C)O
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:19]([cH:21]1)[O:20][C:8](=[O:9])[CH:7]2[c:10]1[cH:11][cH:12][c:13]([CH:14]([CH3:15])[CH3:16])[cH:17][cH:18]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH:7]([CH2:8][OH:9])[c:10]2[cH:11][cH:12][c:13]([CH:14]([CH3:15])[CH3:16])[cH:17][cH:18]2)[c:19]([OH:20])[cH:21]1
Cc1cc(C)c2c(c1)OC(=O)C2c1ccc(C(C)C)cc1
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1
null
null
C(C)(=O)OCC.CCCCCC
Reduction
OtherReaction
da0d3c7a3eeadda28a29d228ff8f103888c428bfcfc295782d2b1143ff8ed39e
bb621eee13e64a87401761367bc299c7ba93ca9330953c6249ee208fbd91494f
c1ccc(Cc2ccccc2)cc1
[O;H0;D1;+0:1]=[C;H0;D3;+0:2]1-[O;H0;D2;+0:3]-[c:4](:[c:5]):[c:6]-[C:7]-1-[c:8]>>[OH;D1;+0:3]-[c:4](:[c:5]):[c:6]-[C:7](-[c:8])-[CH2;D2;+0:2]-[OH;D1;+0:1]
93
[{"value": 93.0, "product": "OCC(C1=CC=C(C=C1)C(C)C)C1=C(C=C(C=C1C)C)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 3-(4-isopropylphenyl)-4,6-dimethyl-1-benzofuran-2(3H)-one synthesized in Reference Example 4, the title compound was synthesized in the same manner as in Reference Example 8. Yield 93%. Melting point: 101-102° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: synthesized in Refe...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol.Aromatic alcohol
c1ccc2c(c1)CCO2
null
c1ccccc1.c1ccccc1
null
C(C)(=O)OCC.CCCCCC
null
null
Cc1cc(C)c2c(c1)OC(=O)C2c1ccc(C(C)C)cc1>C(C)(=O)OCC.CCCCCC>Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-5564278b039e40dd9c6990ea070e14f7
Cc1cc(C)c2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1>>Cc1cc(C)c(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
C(C)(C)C1=CC=C(C=C1)C1(C(OC2=C1C(=CC(=C2C)C)C)=O)C>>OCC(C)(C1=CC=C(C=C1)C(C)C)C1=C(C(=C(C=C1C)C)C)O
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:20]([c:22]1[CH3:23])[O:21][C:9](=[O:10])[C:7]2([CH3:8])[c:11]1[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([C:7]([CH3:8])([CH2:9][OH:10])[c:11]2[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]2)[c:20]([OH:21...
Cc1cc(C)c2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1
Cc1cc(C)c(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
null
null
C(C)(=O)OCC.CCCCCC
Reduction
OtherReaction
da0d3c7a3eeadda28a29d228ff8f103888c428bfcfc295782d2b1143ff8ed39e
bb621eee13e64a87401761367bc299c7ba93ca9330953c6249ee208fbd91494f
c1ccc(Cc2ccccc2)cc1
[C;D1;H3:1]-[C:2]1(-[c:3])-[c:4]:[c:5](:[c:6])-[O;H0;D2;+0:7]-[C;H0;D3;+0:8]-1=[O;H0;D1;+0:9]>>[C;D1;H3:1]-[C:2](-[c:3])(-[CH2;D2;+0:8]-[OH;D1;+0:9])-[c:4]:[c:5](-[OH;D1;+0:7]):[c:6]
83
[{"value": 83.0, "product": "OCC(C)(C1=CC=C(C=C1)C(C)C)C1=C(C(=C(C=C1C)C)C)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 3-(4-isopropylphenyl)-3,4,6,7-tetramethyl-1-benzofuran-2(3H)-one synthesized in Reference Example 6, the title compound was synthesized in the same manner as in Reference Example 8. Yield 83%. Melting point: 116-117° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: synthesized ...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol.Aromatic alcohol
c1ccc2c(c1)CCO2
null
c1ccccc1.c1ccccc1
null
C(C)(=O)OCC.CCCCCC
null
null
Cc1cc(C)c2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1>C(C)(=O)OCC.CCCCCC>Cc1cc(C)c(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-36071a950ced47cc9b3a73d604d452bd
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1C>>Cc1cc(C)c2c(c1C)OCC2c1ccc(C(C)C)cc1
OCC(C1=CC=C(C=C1)C(C)C)C1=C(C(=C(C=C1C)C)C)O.N(=NC(=O)OCC)C(=O)OCC.C1(=CC=CC=C1)C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=CC(=C2C)C)C
O[CH2:11][CH:12]([c:6]1[c:4]([CH3:5])[cH:3][c:2]([CH3:1])[c:8]([CH3:9])[c:7]1[OH:10])[c:13]1[cH:14][cH:15][c:16]([CH:17]([CH3:18])[CH3:19])[cH:20][cH:21]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:7]([c:8]1[CH3:9])[O:10][CH2:11][CH:12]2[c:13]1[cH:14][cH:15][c:16]([CH:17]([CH3:18])[CH3:19])[cH:20][cH:21]1
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1C
Cc1cc(C)c2c(c1C)OCC2c1ccc(C(C)C)cc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether (intramolecular)
08fe01f624cfc4673e7c832ce270800ddccb38ff76736dab6575edf463f51b05
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccc(C2COc3ccccc32)cc1
O-[CH2;D2;+0:1]-[C:2](-[c:3])-[c:4]:[c:5](-[OH;D1;+0:6]):[c:7]>>[c:3]-[C:2]1-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:5](:[c:7]):[c:4]-1
84
[{"value": 84.0, "product": "C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=CC(=C2C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 2-(2-hydroxy-1-(4-isopropylphenyl)ethyl)-3,5,6-trimethylphenol obtained in Reference Example 8 (7.85 g, 26.3 mmol) and triphenylphosphine (7.58 g, 28.9 mmol) in THF (60 mL) was added diethyl azodicarboxylate (a 40% toluene solution, 12.6 g, 28.9 mmol) with ice-cooling, and the mixture was stirred at ro...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
C1CCOC1
null
1
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1C>C1CCOC1>Cc1cc(C)c2c(c1C)OCC2c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-628effa69f664d04b48453bd2748c606
Cc1ccc(C(CO)c2ccc(C(C)C)cc2)c(O)c1C>>Cc1ccc2c(c1C)OCC2c1ccc(C(C)C)cc1
OCC(C1=CC=C(C=C1)C(C)C)C1=CC=C(C(=C1O)C)C>>C(C)(C)C1=CC=C(C=C1)C1COC2=C1C=CC(=C2C)C
O[CH2:10][CH:11]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[c:7]([CH3:8])[c:6]1[OH:9])[c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([c:7]1[CH3:8])[O:9][CH2:10][CH:11]2[c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1
Cc1ccc(C(CO)c2ccc(C(C)C)cc2)c(O)c1C
Cc1ccc2c(c1C)OCC2c1ccc(C(C)C)cc1
null
null
CO
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether (intramolecular)
08fe01f624cfc4673e7c832ce270800ddccb38ff76736dab6575edf463f51b05
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccc(C2COc3ccccc32)cc1
O-[CH2;D2;+0:1]-[C:2](-[c:3])-[c:4]:[c:5](-[OH;D1;+0:6]):[c:7]>>[c:3]-[C:2]1-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:5](:[c:7]):[c:4]-1
80
[{"value": 80.0, "product": "C(C)(C)C1=CC=C(C=C1)C1COC2=C1C=CC(=C2C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 6-(2-hydroxy-1-(4-isopropylphenyl)ethyl)-2,3-dimethylphenol synthesized in Reference Example 9, the title compound was synthesized in the same manner as in Reference Example 13. Yield 80%. Melting point: 50-51° C. (methanol). Conditions: See reaction.notes.procedure_details. Workup: synthesized in Reference Examp...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
CO
null
null
Cc1ccc(C(CO)c2ccc(C(C)C)cc2)c(O)c1C>CO>Cc1ccc2c(c1C)OCC2c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0fb32881f4354a9789f966d985b1b45a
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1>>Cc1cc(C)c2c(c1)OCC2c1ccc(C(C)C)cc1
OCC(C1=CC=C(C=C1)C(C)C)C1=C(C=C(C=C1C)C)O>>C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=CC(=C2)C)C
O[CH2:10][CH:11]([c:6]1[c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:8][c:7]1[OH:9])[c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]2[c:7]([cH:8]1)[O:9][CH2:10][CH:11]2[c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1
Cc1cc(C)c2c(c1)OCC2c1ccc(C(C)C)cc1
null
null
CO
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether (intramolecular)
08fe01f624cfc4673e7c832ce270800ddccb38ff76736dab6575edf463f51b05
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccc(C2COc3ccccc32)cc1
O-[CH2;D2;+0:1]-[C:2](-[c:3])-[c:4]:[c:5](-[OH;D1;+0:6]):[c:7]>>[c:3]-[C:2]1-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:5](:[c:7]):[c:4]-1
85
[{"value": 85.0, "product": "C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=CC(=C2)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2-(2-hydroxy-1-(4-isopropylphenyl)ethyl)-3,5-dimethylphenol synthesized in Reference Example 10, the title compound was synthesized in the same manner as in Reference Example 13. Yield 85%. Melting point: 46-47° C. (methanol). Conditions: See reaction.notes.procedure_details. Workup: synthesized in Reference Exam...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
CO
null
null
Cc1cc(C)c(C(CO)c2ccc(C(C)C)cc2)c(O)c1>CO>Cc1cc(C)c2c(c1)OCC2c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-78f320e788624654b9df79edd1721746
CC(C)c1ccc(C(CO)c2cc(Br)ccc2O)cc1>>CC(C)c1ccc(C2COc3ccc(Br)cc32)cc1
BrC1=CC(=C(C=C1)O)C(CO)C1=CC=C(C=C1)C(C)C>>BrC=1C=CC2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1
O[CH2:9][CH:8]([c:7]1[cH:6][cH:5][c:4]([CH:2]([CH3:1])[CH3:3])[cH:19][cH:18]1)[c:17]1[c:11]([OH:10])[cH:12][cH:13][c:14]([Br:15])[cH:16]1>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH:8]2[CH2:9][O:10][c:11]3[cH:12][cH:13][c:14]([Br:15])[cH:16][c:17]32)[cH:18][cH:19]1
CC(C)c1ccc(C(CO)c2cc(Br)ccc2O)cc1
CC(C)c1ccc(C2COc3ccc(Br)cc32)cc1
null
null
CO
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether (intramolecular)
08fe01f624cfc4673e7c832ce270800ddccb38ff76736dab6575edf463f51b05
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccc(C2COc3ccccc32)cc1
O-[CH2;D2;+0:1]-[C:2](-[c:3])-[c:4]:[c:5](-[OH;D1;+0:6]):[c:7]>>[c:7]:[c:5]1:[c:4]-[C:2](-[c:3])-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-1
62
[{"value": 62.0, "product": "BrC=1C=CC2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 4-bromo-2-(2-hydroxy-1-(4-isopropylphenyl)ethyl)phenol synthesized in Reference Example 11, the title compound was synthesized in the same manner as in Reference Example 13. Yield 62%. Melting point: 90-91° C. (methanol). Conditions: See reaction.notes.procedure_details. Workup: synthesized in Reference Example 1...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
HO-
CO
null
null
CC(C)c1ccc(C(CO)c2cc(Br)ccc2O)cc1>CO>CC(C)c1ccc(C2COc3ccc(Br)cc32)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0ed47b445b744e1f84ecf4da64e12ce0
BrBr.Cc1cc(C)c2c(c1C)OCC2c1ccc(C(C)C)cc1>>Cc1c(C)c2c(c(C)c1Br)C(c1ccc(C(C)C)cc1)CO2
BrBr.C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=CC(=C2C)C)C.O.C(C)(=O)[O-].[Na+]>>BrC=1C(=C(C2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1C)C)C
Br[Br:10].[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[cH:9]1)[CH:11]([c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1)[CH2:21][O:22]2>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[Br:10])[CH:11]([c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1)[CH2:21][...
BrBr.Cc1cc(C)c2c(c1C)OCC2c1ccc(C(C)C)cc1
Cc1c(C)c2c(c(C)c1Br)C(c1ccc(C(C)C)cc1)CO2
null
null
C(C)#N
Functional Group Interconversion
Bromination
8a5899f39c577ae2f5dbb7e89484f9814910050aa00e810b5c8bafb1acd06dbc
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc(C2COc3ccccc32)cc1
Br-[Br;H0;D1;+0:1].[C;D1;H3:2]-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6](-[C;D1;H3:7]):[c:8]>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:5](:[c:3](-[C;D1;H3:2]):[c:4]):[c:6](-[C;D1;H3:7]):[c:8]
99
[{"value": 99.0, "product": "BrC=1C(=C(C2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a mixture of 3-(4-isopropylphenyl)-4,6,7-trimethyl-2,3-dihydro-1-benzofuran synthesized in Reference Example 13 (6.10 g, 21.8 mmol) and sodium acetate (1.97 g, 24.0 mmol) in acetonitrile (30 mL) was added bromine (1.17 mL, 22.9 mmol), and the mixture was stirred at the same temperature for 1 hour. Water was poured i...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
HBr
C(C)#N
null
1
BrBr.Cc1cc(C)c2c(c1C)OCC2c1ccc(C(C)C)cc1>C(C)#N>Cc1c(C)c2c(c(C)c1Br)C(c1ccc(C(C)C)cc1)CO2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-72240799120b43f39ccf3ee7fbeb78a0
Cc1c(Br)cc2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1>>Cc1c(Br)cc(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
BrC=1C(=C(C2=C(C(C(O2)=O)(C)C2=CC=C(C=C2)C(C)C)C1)C)C>>BrC1=C(C(=C(C(=C1)C(CO)(C)C1=CC=C(C=C1)C(C)C)O)C)C
[CH3:1][c:2]1[c:3]([Br:4])[cH:5][c:6]2[c:20]([c:22]1[CH3:23])[O:21][C:9](=[O:10])[C:7]2([CH3:8])[c:11]1[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]1>>[CH3:1][c:2]1[c:3]([Br:4])[cH:5][c:6]([C:7]([CH3:8])([CH2:9][OH:10])[c:11]2[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]2)[c:20]([OH:21])...
Cc1c(Br)cc2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1
Cc1c(Br)cc(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
null
null
C(C)(=O)OCC.CCCCCC
Reduction
OtherReaction
da0d3c7a3eeadda28a29d228ff8f103888c428bfcfc295782d2b1143ff8ed39e
bb621eee13e64a87401761367bc299c7ba93ca9330953c6249ee208fbd91494f
c1ccc(Cc2ccccc2)cc1
[C;D1;H3:1]-[C:2]1(-[c:3])-[c:4]:[c:5](:[c:6])-[O;H0;D2;+0:7]-[C;H0;D3;+0:8]-1=[O;H0;D1;+0:9]>>[C;D1;H3:1]-[C:2](-[c:3])(-[CH2;D2;+0:8]-[OH;D1;+0:9])-[c:4]:[c:5](-[OH;D1;+0:7]):[c:6]
83
[{"value": 83.0, "product": "BrC1=C(C(=C(C(=C1)C(CO)(C)C1=CC=C(C=C1)C(C)C)O)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 5-bromo-3-(4-isopropylphenyl)-3,6,7-trimethyl-1-benzofuran-2(3H)-one synthesized in Reference Example 21, the title compound was synthesized in the same manner as in Reference Example 8. Yield 83%. Melting point: 110-111° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: synthes...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol.Aromatic alcohol
c1ccc2c(c1)CCO2
null
c1ccccc1.c1ccccc1
null
C(C)(=O)OCC.CCCCCC
null
null
Cc1c(Br)cc2c(c1C)OC(=O)C2(C)c1ccc(C(C)C)cc1>C(C)(=O)OCC.CCCCCC>Cc1c(Br)cc(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-e203dee6114543f08770ce76990bd0d0
Cc1c(C)c2c(c(C)c1Br)C(c1ccc(C(C)C)cc1)CO2.NCc1ccccc1>>Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(c1ccc(C(C)C)cc1)CO2
BrC=1C(=C(C2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1C)C)C.O.C(C1=CC=CC=C1)N.CC(C)([O-])C.[Na+]>>C(C1=CC=CC=C1)NC=1C(=C(C2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1C)C)C
Br[c:9]1[c:2]([CH3:1])[c:3]([CH3:4])[c:5]2[c:6]([c:7]1[CH3:8])[CH:18]([c:19]1[cH:20][cH:21][c:22]([CH:23]([CH3:24])[CH3:25])[cH:26][cH:27]1)[CH2:28][O:29]2.[NH2:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][cH:16][cH:17]1>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH:10][CH2:11][c:12]1[cH:13][cH:14][cH:15][...
Cc1c(C)c2c(c(C)c1Br)C(c1ccc(C(C)C)cc1)CO2.NCc1ccccc1
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(c1ccc(C(C)C)cc1)CO2
null
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C=1C=CC(=CC1)P(C=2C=CC=CC2)C3=CC=C4C=CC=CC4=C3C5=C6C=CC=CC6=CC=C5P(C=7C=CC=CC7)C=8C=CC=CC8
C1(=CC=CC=C1)C
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
3eefa8c0242a0dbc67760ed46fbbe572c7b05262288867a6644b519cc5731092
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2ccc3c(c2)C(c2ccccc2)CO3)cc1
Br-[c;H0;D3;+0:1](:[c:2](-[C;D1;H3:3]):[c:4]):[c:5](-[C;D1;H3:6]):[c:7].[NH2;D1;+0:8]-[C:9]-[c:10]>>[C;D1;H3:3]-[c:2](:[c:4]):[c;H0;D3;+0:1](-[NH;D2;+0:8]-[C:9]-[c:10]):[c:5](-[C;D1;H3:6]):[c:7]
91
[{"value": 91.0, "product": "C(C1=CC=CC=C1)NC=1C(=C(C2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To a solution of 5-bromo-3-(4-isopropylphenyl)-4,6,7-trimethyl-2,3-dihydro-1-benzofuran obtained in Reference Example 18 (920 mg, 2.56 mmol) and benzylamine (0.34 mL, 3.07 mmol) in toluene (10 mL), were added palladium acetate (6 mg, 0.03 mmol) and BINAP (48 mg, 0.09 mmol) at room temperature, and the mixture was stirr...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
c1ccccc1.c1ccccc1.c1ccc2c(c1)CCO2
HBr
C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C=1C=CC(=CC1)P(C=2C=CC=CC2)C3=CC=C4C=CC=CC4=C3C5=C6C=CC=CC6=CC=C5P(C=7C=CC=CC7)C=8C=CC=CC8.C1(=CC=CC=C1)C
null
0.25
Cc1c(C)c2c(c(C)c1Br)C(c1ccc(C(C)C)cc1)CO2.NCc1ccccc1>C(C)(=O)[O-].[Pd+2].C(C)(=O)[O-].C=1C=CC(=CC1)P(C=2C=CC=CC2)C3=CC=C4C=CC=CC4=C3C5=C6C=CC=CC6=CC=C5P(C=7C=CC=CC7)C=8C=CC=CC8.C1(=CC=CC=C1)C>Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(c1ccc(C(C)C)cc1)CO2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ebf80d70ffce43bea7334ade08b99f29
Cc1c(Br)cc(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C>>Cc1c(Br)cc2c(c1C)OCC2(C)c1ccc(C(C)C)cc1
BrC1=C(C(=C(C(=C1)C(CO)(C)C1=CC=C(C=C1)C(C)C)O)C)C.N(=NC(=O)OCC)C(=O)OCC.C1(=CC=CC=C1)C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1>>BrC=1C(=C(C2=C(C(CO2)(C)C2=CC=C(C=C2)C(C)C)C1)C)C
O[CH2:11][C:12]([c:6]1[cH:5][c:3]([Br:4])[c:2]([CH3:1])[c:8]([CH3:9])[c:7]1[OH:10])([CH3:13])[c:14]1[cH:15][cH:16][c:17]([CH:18]([CH3:19])[CH3:20])[cH:21][cH:22]1>>[CH3:1][c:2]1[c:3]([Br:4])[cH:5][c:6]2[c:7]([c:8]1[CH3:9])[O:10][CH2:11][C:12]2([CH3:13])[c:14]1[cH:15][cH:16][c:17]([CH:18]([CH3:19])[CH3:20])[cH:21][cH:22...
Cc1c(Br)cc(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C
Cc1c(Br)cc2c(c1C)OCC2(C)c1ccc(C(C)C)cc1
null
null
C1CCOC1
Heteroatom Alkylation and Arylation
Mitsunobu aryl ether (intramolecular)
08fe01f624cfc4673e7c832ce270800ddccb38ff76736dab6575edf463f51b05
2258bd14c3b5449b92dc09cf9fa522f88d5071b4af20f7e968b60aa1ae6db0cf
c1ccc(C2COc3ccccc32)cc1
O-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])(-[c:4])-[c:5]:[c:6](-[OH;D1;+0:7]):[c:8]>>[C;D1;H3:3]-[C:2]1(-[c:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:7]-[c:6](:[c:8]):[c:5]-1
null
[]
null
null
1
HOUR
To a solution of 4-bromo-6-(2-hydroxy-1-(4-isopropylphenyl)-1-methylethyl)-2,3-dimethylphenol obtained in Reference Example 22 (830 mg, 2.21 mmol) and triphenylphosphine (638 mg, 2.43 mmol) in THF (60 mL) was added diethyl azodicarboxylate (a 40% toluene solution, 1.06 g, 2.43 mmol) with ice-cooling, and the mixture wa...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Aromatic alcohol
Ether
null
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
HO-
C1CCOC1
null
1
Cc1c(Br)cc(C(C)(CO)c2ccc(C(C)C)cc2)c(O)c1C>C1CCOC1>Cc1c(Br)cc2c(c1C)OCC2(C)c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-347826c140b148cbaa952a0c62b9a9c0
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(c1ccc(C(C)C)cc1)CO2>>Cc1c(C)c2c(c(C)c1N)C(c1ccc(C(C)C)cc1)CO2
C(C1=CC=CC=C1)NC=1C(=C(C2=C(C(CO2)C2=CC=C(C=C2)C(C)C)C1C)C)C.C(=O)[O-].[NH4+]>>C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=C(C(=C2C)C)N)C
c1ccc(C[NH:10][c:9]2[c:2]([CH3:1])[c:3]([CH3:4])[c:5]3[c:6]([c:7]2[CH3:8])[CH:11]([c:12]2[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]2)[CH2:21][O:22]3)cc1>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH2:10])[CH:11]([c:12]1[cH:13][cH:14][c:15]([CH:16]([CH3:17])[CH3:18])[cH:19][cH:20]1)[...
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(c1ccc(C(C)C)cc1)CO2
Cc1c(C)c2c(c(C)c1N)C(c1ccc(C(C)C)cc1)CO2
null
[C].[Pd]
C(C)O
Deprotection
OtherReaction
93c46c2f9981b731115295839d7158a8a73faedd00707b7604ace2fa5f580cbc
f6571fb5b7780a2b467937abfba91ba7d787f19d503265f299ff4a25a08963bd
c1ccc(C2COc3ccccc32)cc1
[c:1]:[c:2](-[NH;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]>>[NH2;D1;+0:3]-[c:2](:[c:1]):[c:4]
74
[{"value": 74.0, "product": "C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=C(C(=C2C)C)N)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of N-benzyl-3-(4-isopropylphenyl)-4,6,7-trimethyl-2,3-dihydro-1-benzofuran-5-amine obtained in Reference Example 24 (900 mg, 2.33 mmol), 10%-palladium carbon (50% hydrous, 90 mg) and ammonium formate (294 mg, 4.66 mmol) in ethanol (10 mL) was heated under reflux for 2 hours. The solid material was removed and...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Primary amine
c1ccccc1
null
c1ccccc1.c1ccc2c(c1)CCO2
Other
[C].[Pd].C(C)O
null
null
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(c1ccc(C(C)C)cc1)CO2>[C].[Pd].C(C)O>Cc1c(C)c2c(c(C)c1N)C(c1ccc(C(C)C)cc1)CO2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a303b20a472c4e51902ab574154039c7
CCOC(=O)C(C)(C)Br.Cc1cccc(O)c1C>>CCOC(=O)C(C)(C)Oc1cccc(C)c1C
O.CC1=C(C=CC=C1C)O.BrC(C(=O)OCC)(C)C.C([O-])([O-])=O.[K+].[K+]>>CC1=C(OC(C(=O)OCC)(C)C)C=CC=C1C
Br[C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8].[OH:9][c:10]1[cH:11][cH:12][cH:13][c:14]([CH3:15])[c:16]1[CH3:17]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[O:9][c:10]1[cH:11][cH:12][cH:13][c:14]([CH3:15])[c:16]1[CH3:17]
CCOC(=O)C(C)(C)Br.Cc1cccc(O)c1C
CCOC(=O)C(C)(C)Oc1cccc(C)c1C
null
null
CS(=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
657b1e065fabda84e4d6cc80f4d94ce754af0792c9117981e41887a4384f6981
2495a256265ef36132d409a6a3e2bd04c3acda5f236d910f184b0a36a846defe
c1ccccc1
Br-[C;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](=[O;D1;H0:5])-[#8:6]-[C:7].[OH;D1;+0:8]-[c:9](:[c:10]):[c:11]>>[C:7]-[#8:6]-[C:4](=[O;D1;H0:5])-[C;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[O;H0;D2;+0:8]-[c:9](:[c:10]):[c:11]
null
[]
null
null
36
HOUR
To a solution of 2,3-dimethylphenol (25.0 g, 205 mmol) in dimethylsulfoxide (200 mL) were added ethyl 2-bromo-isobutyrate (60 mL, 409 mmol) and potassium carbonate (56.5 g, 409 mmol) at room temperature, and the mixture was stirred for 36 hours. Water was added to the reaction solution and the mixture was extracted wit...
10.6084/m9.figshare.5104873.v1
null
Tertiary halide.Ester.Aromatic alcohol
Ester.Ether
null
null
c1ccccc1
HBr
CS(=O)C
null
36
CCOC(=O)C(C)(C)Br.Cc1cccc(O)c1C>CS(=O)C>CCOC(=O)C(C)(C)Oc1cccc(C)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-6ce2883d770d4f568bd1cdc173c6f12e
Cc1cccc(OC(C)(C)C(=O)O)c1C>>Cc1ccc2c(c1C)OC(C)(C)C2=O
CC1=C(OC(C(=O)O)(C)C)C=CC=C1C.[Cl-].[Al+3].[Cl-].[Cl-].CN(C)C=O.C(C(=O)Cl)(=O)Cl>>CC1(OC2=C(C1=O)C=CC(=C2C)C)C
O[C:13]([C:10]([O:9][c:6]1[cH:5][cH:4][cH:3][c:2]([CH3:1])[c:7]1[CH3:8])([CH3:11])[CH3:12])=[O:14]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]2[c:6]([c:7]1[CH3:8])[O:9][C:10]([CH3:11])([CH3:12])[C:13]2=[O:14]
Cc1cccc(OC(C)(C)C(=O)O)c1C
Cc1ccc2c(c1C)OC(C)(C)C2=O
null
null
O.C1CCOC1
Functional Group Interconversion
OtherReaction
07c0617fba4b5b8b4f6e211c6b50ebf5bf60539aad6b1d235a93c13cf5d42336
6a71bb5a71b59feeb4f6a39b1b66fa450a058b64b0a3909e1a51c22473a141c5
O=C1COc2ccccc21
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[#8:6]-[c:7](:[c:8]):[cH;D2;+0:9]:[c:10]:[c:11]>>[C;D1;H3:4]-[C:3]1(-[C;D1;H3:5])-[#8:6]-[c:7](:[c:8]):[c;H0;D3;+0:9](:[c:10]:[c:11])-[C;H0;D3;+0:1]-1=[O;D1;H0:2]
71
[{"value": 71.0, "product": "CC1(OC2=C(C1=O)C=CC(=C2C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 2-(2,3-dimethylphenoxy)-2-methylpropionic acid obtained in Reference Example 36 (21.0 g, 101 mmol) in THF (200 mL) was added DMF (0.1 mL), and then to the mixture was added dropwise oxalyl chloride (10.6 mL, 121 mmol). The reaction solution was warmed to room temperature, stirred for 1 hour, and then c...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ketone
c1ccccc1
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
HO-
O.C1CCOC1
null
1
Cc1cccc(OC(C)(C)C(=O)O)c1C>O.C1CCOC1>Cc1ccc2c(c1C)OC(C)(C)C2=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-b16d625f2845495d85c3041906b21fcb
Cc1cc(OC(C)(C)C(=O)O)cc(C)c1C>>Cc1cc2c(c(C)c1C)C(=O)C(C)(C)O2
CC=1C=C(OC(C(=O)O)(C)C)C=C(C1C)C>>CC1(OC2=C(C1=O)C(=C(C(=C2)C)C)C)C
O[C:10](=[O:11])[C:12]([CH3:13])([CH3:14])[O:15][c:4]1[cH:3][c:2]([CH3:1])[c:8]([CH3:9])[c:6]([CH3:7])[cH:5]1>>[CH3:1][c:2]1[cH:3][c:4]2[c:5]([c:6]([CH3:7])[c:8]1[CH3:9])[C:10](=[O:11])[C:12]([CH3:13])([CH3:14])[O:15]2
Cc1cc(OC(C)(C)C(=O)O)cc(C)c1C
Cc1cc2c(c(C)c1C)C(=O)C(C)(C)O2
null
null
CCCCCC
Functional Group Interconversion
OtherReaction
07c0617fba4b5b8b4f6e211c6b50ebf5bf60539aad6b1d235a93c13cf5d42336
6a71bb5a71b59feeb4f6a39b1b66fa450a058b64b0a3909e1a51c22473a141c5
O=C1COc2ccccc21
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])(-[C;D1;H3:5])-[#8:6]-[c:7](:[c:8]):[cH;D2;+0:9]:[c:10](-[C;D1;H3:11]):[c:12]>>[C;D1;H3:4]-[C:3]1(-[C;D1;H3:5])-[#8:6]-[c:7](:[c:8]):[c;H0;D3;+0:9](:[c:10](-[C;D1;H3:11]):[c:12])-[C;H0;D3;+0:1]-1=[O;D1;H0:2]
90
[{"value": 90.0, "product": "CC1(OC2=C(C1=O)C(=C(C(=C2)C)C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2-(3,4,5-trimethyl phenoxy)-2-methylpropionic acid obtained in Reference Example 40, the title compound was synthesized in the same manner as in Reference Example 41. Yield 90%. Melting point: 77-78° C. (hexane). Conditions: See reaction.notes.procedure_details. Workup: obtained in Reference Example 40
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ketone
c1ccccc1
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
HO-
CCCCCC
null
null
Cc1cc(OC(C)(C)C(=O)O)cc(C)c1C>CCCCCC>Cc1cc2c(c(C)c1C)C(=O)C(C)(C)O2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bf5133e21aff459ca5e01da7ef38cae1
Cc1c([N+](=O)[O-])cc2c(c1C)OC(C)(C)C2=O>>Cc1c(N)cc2c(c1C)OC(C)(C)C2=O
CC1(OC2=C(C1=O)C=C(C(=C2C)C)[N+](=O)[O-])C.C(=O)[O-].[NH4+]>>NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1)C)C
O=[N+:4]([O-])[c:3]1[c:2]([CH3:1])[c:8]([CH3:9])[c:7]2[c:6]([cH:5]1)[C:14](=[O:15])[C:11]([CH3:12])([CH3:13])[O:10]2>>[CH3:1][c:2]1[c:3]([NH2:4])[cH:5][c:6]2[c:7]([c:8]1[CH3:9])[O:10][C:11]([CH3:12])([CH3:13])[C:14]2=[O:15]
Cc1c([N+](=O)[O-])cc2c(c1C)OC(C)(C)C2=O
Cc1c(N)cc2c(c1C)OC(C)(C)C2=O
null
[C].[Pd]
CO
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C1COc2ccccc21
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
92
[{"value": 92.0, "product": "NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 2,2,6,7-tetramethyl-5-nitro-1-benzofuran-3(2H)-one obtained in Reference Example 46 (5.0 g, 21.3 mmol), 10%-palladium carbon (50% hydrous, 500 mg) and ammonium formate (7.06 g, 85.0 mmol) in methanol (100 mL) was heated under reflux for two hours. The solid material was removed and the filtrate was concent...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2c(c1)CCO2
Other
[C].[Pd].CO
null
null
Cc1c([N+](=O)[O-])cc2c(c1C)OC(C)(C)C2=O>[C].[Pd].CO>Cc1c(N)cc2c(c1C)OC(C)(C)C2=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ac71fe16686444ff81ae363612198b6f
Cc1cc([N+](=O)[O-])c(C)c2c1OC(C)(C)C2=O>>Cc1cc(N)c(C)c2c1OC(C)(C)C2=O
CC1(OC2=C(C1=O)C(=C(C=C2C)[N+](=O)[O-])C)C>>NC=1C=C(C2=C(C(C(O2)(C)C)=O)C1C)C
O=[N+:5]([O-])[c:4]1[cH:3][c:2]([CH3:1])[c:9]2[c:8]([c:6]1[CH3:7])[C:14](=[O:15])[C:11]([CH3:12])([CH3:13])[O:10]2>>[CH3:1][c:2]1[cH:3][c:4]([NH2:5])[c:6]([CH3:7])[c:8]2[c:9]1[O:10][C:11]([CH3:12])([CH3:13])[C:14]2=[O:15]
Cc1cc([N+](=O)[O-])c(C)c2c1OC(C)(C)C2=O
Cc1cc(N)c(C)c2c1OC(C)(C)C2=O
null
null
C(C)(=O)OCC.CCCCCC
Reduction
Reduction of nitro groups to amines
bbc242b150a51e69d3ad1caaa391f4422710431b398dcb880555f476706790be
7b0317532ea57a4fcedc1efc3e3c22eb5238d1c8330da53d4f9801fc2391f567
O=C1COc2ccccc21
O=[N+;H0;D3:1](-[O-])-[c:2](:[c:3]):[c:4]>>[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]
97
[{"value": 97.0, "product": "NC=1C=C(C2=C(C(C(O2)(C)C)=O)C1C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2,2,4,7-tetramethyl-5-nitro-1-benzofuran-3(2H)-one obtained in Reference Example 47, the title compound was synthesized in the same manner as in Reference Example 54. Yield 97%. Melting point: 124-126° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: obtained in Reference Examp...
10.6084/m9.figshare.5104873.v1
null
Nitro group
Primary amine
null
null
c1ccc2c(c1)CCO2
Other
C(C)(=O)OCC.CCCCCC
null
null
Cc1cc([N+](=O)[O-])c(C)c2c1OC(C)(C)C2=O>C(C)(=O)OCC.CCCCCC>Cc1cc(N)c(C)c2c1OC(C)(C)C2=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d23742b8602f40599e8257802fb962e1
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(=O)C(C)(C)O2>>Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2
C(C1=CC=CC=C1)NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C>>NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C
c1ccc(C[NH:10][c:9]2[c:2]([CH3:1])[c:3]([CH3:4])[c:5]3[c:6]([c:7]2[CH3:8])[C:11](=[O:12])[C:13]([CH3:14])([CH3:15])[O:16]3)cc1>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH2:10])[C:11](=[O:12])[C:13]([CH3:14])([CH3:15])[O:16]2
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(=O)C(C)(C)O2
Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2
null
null
C(C)(=O)OCC.CCCCCC
Deprotection
OtherReaction
93c46c2f9981b731115295839d7158a8a73faedd00707b7604ace2fa5f580cbc
f6571fb5b7780a2b467937abfba91ba7d787f19d503265f299ff4a25a08963bd
O=C1COc2ccccc21
[c:1]:[c:2](-[NH;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]>>[NH2;D1;+0:3]-[c:2](:[c:1]):[c:4]
88
[{"value": 88.0, "product": "NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 5-(benzylamino)-2,2,4,6,7-pentamethyl-1-benzofuran-3(2H)-one obtained in Reference Example 52, the title compound was synthesized in the same manner as in Reference Example 30. Yield 88%. Melting point: 92-93° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: obtained in Referen...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Primary amine
c1ccccc1
null
c1ccc2c(c1)CCO2
Other
C(C)(=O)OCC.CCCCCC
null
null
Cc1c(C)c2c(c(C)c1NCc1ccccc1)C(=O)C(C)(C)O2>C(C)(=O)OCC.CCCCCC>Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-32c37e0b60494dd7b26c55a4580caac5
Cc1c(C)c(NCc2ccccc2)c2c(c1C)C(=O)C(C)(C)O2>>Cc1c(C)c(N)c2c(c1C)C(=O)C(C)(C)O2
C(C1=CC=CC=C1)NC1=C(C(=C(C=2C(C(OC21)(C)C)=O)C)C)C>>NC1=C(C(=C(C=2C(C(OC21)(C)C)=O)C)C)C
c1ccc(C[NH:6][c:5]2[c:3]([CH3:4])[c:2]([CH3:1])[c:9]([CH3:10])[c:8]3[c:7]2[O:16][C:13]([CH3:14])([CH3:15])[C:11]3=[O:12])cc1>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]([NH2:6])[c:7]2[c:8]([c:9]1[CH3:10])[C:11](=[O:12])[C:13]([CH3:14])([CH3:15])[O:16]2
Cc1c(C)c(NCc2ccccc2)c2c(c1C)C(=O)C(C)(C)O2
Cc1c(C)c(N)c2c(c1C)C(=O)C(C)(C)O2
null
null
C(C)(=O)OCC.CCCCCC
Deprotection
OtherReaction
93c46c2f9981b731115295839d7158a8a73faedd00707b7604ace2fa5f580cbc
f6571fb5b7780a2b467937abfba91ba7d787f19d503265f299ff4a25a08963bd
O=C1COc2ccccc21
[#8:1]-[c:2]:[c:3](-[NH;D2;+0:4]-C-c1:c:c:c:c:c:1):[c:5]>>[#8:1]-[c:2]:[c:3](-[NH2;D1;+0:4]):[c:5]
null
[]
null
null
null
null
Using 7-(benzylamino)-2,2,4,5,6-pentamethyl-1-benzofuran-3(2H)-one obtained in Reference Example 53, the title compound was synthesized in the same manner as in Reference Example 30. Yield: quantitative. Melting point: 141-142° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: obtaine...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Primary amine
c1ccccc1
null
c1ccc2c(c1)CCO2
Other
C(C)(=O)OCC.CCCCCC
null
null
Cc1c(C)c(NCc2ccccc2)c2c(c1C)C(=O)C(C)(C)O2>C(C)(=O)OCC.CCCCCC>Cc1c(C)c(N)c2c(c1C)C(=O)C(C)(C)O2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d1c388f8cd154e7aa4759a6e8dabdd25
CC(C)(C)CC(=O)Cl.Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2>>Cc1c(C)c2c(c(C)c1NC(=O)CC(C)(C)C)C(=O)C(C)(C)O2
C(C)N(CC)CC.NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C.O.C(C)(C)(C)CC(=O)Cl>>CC(CC(=O)NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C)(C)C
Cl[C:11](=[O:12])[CH2:13][C:14]([CH3:15])([CH3:16])[CH3:17].[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH2:10])[C:18](=[O:19])[C:20]([CH3:21])([CH3:22])[O:23]2>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH:10][C:11](=[O:12])[CH2:13][C:14]([CH3:15])([CH3:16])[CH3:17])[C:18](=[O:19])[C:...
CC(C)(C)CC(=O)Cl.Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2
Cc1c(C)c2c(c(C)c1NC(=O)CC(C)(C)C)C(=O)C(C)(C)O2
null
null
ClCCl
Acylation
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
38143a4d536201990008fd6f2c68e6571a341d1c367481869fbbbe36cb038937
0e6ae078978e324f714e184b4f72826d4e3bf2d9ab22d6e9f73740af687be16f
O=C1COc2ccccc21
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
54
[{"value": 54.0, "product": "CC(CC(=O)NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 5-amino-2,2,4,6,7-pentamethyl-1-benzofuran-3(2H)-one obtained in Reference Example 57 (3.00 g, 13.7 mmol) and tert-butylacetyl chloride (2.03 g, 15.1 mmol) in dichloromethane (30 mL) was added triethylamine (2.3 mL, 16.4 mmol) at room temperature, and the mixture was stirred at room temperature for 30 ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Primary amine
Secondary amide
null
null
c1ccc2c(c1)CCO2
HCl
ClCCl
null
0.5
CC(C)(C)CC(=O)Cl.Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2>ClCCl>Cc1c(C)c2c(c(C)c1NC(=O)CC(C)(C)C)C(=O)C(C)(C)O2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a4969a7af16644b7a01aa9a3133f17ea
Cc1c(C)c2c(c(C)c1N)OC(C)(C)C2=O.O=CO>>Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2=O
NC1=C(C2=C(C(C(O2)(C)C)=O)C(=C1C)C)C.C(=O)O>>CC1(OC2=C(C1=O)C(=C(C(=C2C)NC=O)C)C)C
[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH2:10])[O:13][C:14]([CH3:15])([CH3:16])[C:17]2=[O:18].O[CH:11]=[O:12]>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH:10][CH:11]=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[C:17]2=[O:18]
Cc1c(C)c2c(c(C)c1N)OC(C)(C)C2=O.O=CO
Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2=O
null
null
null
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C1COc2ccccc21
O-[CH;D2;+0:1]=[O;D1;H0:2].[NH2;D1;+0:3]-[c:4](:[c:5]):[c:6]>>[O;D1;H0:2]=[CH;D2;+0:1]-[NH;D2;+0:3]-[c:4](:[c:5]):[c:6]
81
[{"value": 81.0, "product": "CC1(OC2=C(C1=O)C(=C(C(=C2C)NC=O)C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of formic acid (5 mL) with 6-amino-2,2,4,5,7-pentamethyl-1-benzofuran-3(2H)-one (700 mg, 3.19 mmol) obtained in Reference Example 72, was heated under reflux for 5 hours. The solvent was distilled off under reduced pressure, water and ethyl acetate were added to the residue, and the aqueous layer was extracte...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccc2c(c1)CCO2
HO-
null
null
null
Cc1c(C)c2c(c(C)c1N)OC(C)(C)C2=O.O=CO>>Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2=O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d56a2f205fb14ed195d7ae398bd709e5
CC(C)c1ccc(Br)cc1.Cc1c(NC(=O)OC(C)(C)C)cc2c(c1C)OC(C)(C)C2=O>>Cc1c(NC(=O)OC(C)(C)C)cc2c(c1C)OC(C)(C)C2(O)c1ccc(C(C)C)cc1
CC1(OC2=C(C1=O)C=C(C(=C2C)C)NC(OC(C)(C)C)=O)C.BrC1=CC=C(C=C1)C(C)C.C(CCC)[Li].CCCCCC>>OC1(C(OC2=C1C=C(C(=C2C)C)NC(OC(C)(C)C)=O)(C)C)C2=CC=C(C=C2)C(C)C
Br[c:23]1[cH:24][cH:25][c:26]([CH:27]([CH3:28])[CH3:29])[cH:30][cH:31]1.[CH3:1][c:2]1[c:3]([NH:4][C:5](=[O:6])[O:7][C:8]([CH3:9])([CH3:10])[CH3:11])[cH:12][c:13]2[c:14]([c:15]1[CH3:16])[O:17][C:18]([CH3:19])([CH3:20])[C:21]2=[O:22]>>[CH3:1][c:2]1[c:3]([NH:4][C:5](=[O:6])[O:7][C:8]([CH3:9])([CH3:10])[CH3:11])[cH:12][c:1...
CC(C)c1ccc(Br)cc1.Cc1c(NC(=O)OC(C)(C)C)cc2c(c1C)OC(C)(C)C2=O
Cc1c(NC(=O)OC(C)(C)C)cc2c(c1C)OC(C)(C)C2(O)c1ccc(C(C)C)cc1
null
null
O.C1CCOC1
C-C Coupling
Grignard_alcohol
dc15c67ee64d6e57d57db2cb0f918b6b1d8338f80afda9b1c0093977e8b590e6
b8801be51258f6ee39fb6aad45dd9677b1b9eed3d6e0018ffb065bca8e787abf
c1ccc(C2COc3ccccc32)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C;D1;H3:6]-[C:7]1(-[C;D1;H3:8])-[#8:9]-[c:10]:[c:11](:[c:12])-[C;H0;D3;+0:13]-1=[O;H0;D1;+0:14]>>[C;D1;H3:6]-[C:7]1(-[C;D1;H3:8])-[#8:9]-[c:10]:[c:11](:[c:12])-[C;H0;D4;+0:13]-1(-[OH;D1;+0:14])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
null
[]
null
null
30
MINUTE
To a solution of 4-bromocumene (6.25 g, 31.4 mmol) in THF (50 mL) was added dropwise a solution of n-butyllithium in hexane (1.60 M, 19.6 mL, 31.4 mmol) under arogon atmosphere at −78° C., and the mixture was stirred at the same temperature for 30 minutes. Then, to the reaction solution was added dropwise a solution of...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ketone
Tertiary alcohol
c1ccccc1.c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
c1ccc2c(c1)CCO2.c1ccccc1
Br-
O.C1CCOC1
null
0.5
CC(C)c1ccc(Br)cc1.Cc1c(NC(=O)OC(C)(C)C)cc2c(c1C)OC(C)(C)C2=O>O.C1CCOC1>Cc1c(NC(=O)OC(C)(C)C)cc2c(c1C)OC(C)(C)C2(O)c1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-9063f10311cc4914932d0286636984e3
Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2=O.[Cl][Mg][CH2]c1ccccc1>>Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2(O)Cc1ccccc1
O.C(C1=CC=CC=C1)[Mg]Cl.CC1(OC2=C(C1=O)C(=C(C(=C2C)NC=O)C)C)C>>C(C1=CC=CC=C1)C1(C(OC2=C1C(=C(C(=C2C)NC=O)C)C)(C)C)O
[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH:10][CH:11]=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[C:17]2=[O:18].[Cl][Mg][CH2:19][c:20]1[cH:21][cH:22][cH:23][cH:24][cH:25]1>>[CH3:1][c:2]1[c:3]([CH3:4])[c:5]2[c:6]([c:7]([CH3:8])[c:9]1[NH:10][CH:11]=[O:12])[O:13][C:14]([CH3:15])([CH3:16])[C:17]2([OH:18])[C...
Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2=O.[Cl][Mg][CH2]c1ccccc1
Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2(O)Cc1ccccc1
null
null
C1CCOC1
C-C Coupling
Grignard from ketone to alcohol
2dc8a1a24dc81b7eec00983b8472223608c7deab57f56f9cccd0d6ef8c288a6a
5854166cd4ea706bc07d74dc79eb8f4a990bc6c5eacbf0ca947d88ee86e78fdf
c1ccc(CC2COc3ccccc32)cc1
[C;D1;H3:1]-[C:2]1(-[C;D1;H3:3])-[#8:4]-[c:5]:[c:6](:[c:7])-[C;H0;D3;+0:8]-1=[O;H0;D1;+0:9].[Cl]-[Mg]-[CH2;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[C;D1;H3:1]-[C:2]1(-[C;D1;H3:3])-[#8:4]-[c:5]:[c:6](:[c:7])-[C;H0;D4;+0:8]-1(-[OH;D1;+0:9])-[CH2;D2;+0:10]-[c:11](:[c:12]):[c:13]
null
[]
null
null
2
HOUR
A solution of (2,2,4,5,7-pentamethyl-3-oxo-2,3-dihydro-1-benzofuran-6-yl)formamide obtained in Reference Example 73 (600 mg, 2.43 mmol) in THF (5 mL) was added dropwise to a solution of benzylmagnesium chloride (a 2.0 M THF solution, 10.0 mL, 20.0 mmol) in THF (20 mL) under argon atmosphere, and the mixture was stirred...
10.6084/m9.figshare.5104873.v1
null
Magnesium halide.Ketone
Tertiary alcohol
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2.c1ccccc1
Mg
C1CCOC1
null
2
Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2=O.[Cl][Mg][CH2]c1ccccc1>C1CCOC1>Cc1c(C)c2c(c(C)c1NC=O)OC(C)(C)C2(O)Cc1ccccc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-29548313b0fb41a0930c87c7d862c48a
Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2.Cc1ccc(Br)cc1>>Cc1ccc(C2(O)c3c(C)c(N)c(C)c(C)c3OC2(C)C)cc1
NC=1C(=C(C2=C(C(C(O2)(C)C)=O)C1C)C)C.BrC1=CC=C(C=C1)C.C(CCC)[Li].CCCCCC>>NC=1C(=C(C2=C(C(C(O2)(C)C)(O)C2=CC=C(C=C2)C)C1C)C)C
[C:6]1(=[O:7])[c:8]2[c:9]([CH3:10])[c:11]([NH2:12])[c:13]([CH3:14])[c:15]([CH3:16])[c:17]2[O:18][C:19]1([CH3:20])[CH3:21].Br[c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:23][cH:22]1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6]2([OH:7])[c:8]3[c:9]([CH3:10])[c:11]([NH2:12])[c:13]([CH3:14])[c:15]([CH3:16])[c:17]3[O:18][C:19]2([CH3:20])[CH...
Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2.Cc1ccc(Br)cc1
Cc1ccc(C2(O)c3c(C)c(N)c(C)c(C)c3OC2(C)C)cc1
null
null
O.C1CCOC1
C-C Coupling
Grignard_alcohol
dc15c67ee64d6e57d57db2cb0f918b6b1d8338f80afda9b1c0093977e8b590e6
b8801be51258f6ee39fb6aad45dd9677b1b9eed3d6e0018ffb065bca8e787abf
c1ccc(C2COc3ccccc32)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[C;D1;H3:6]-[C:7]1(-[C;D1;H3:8])-[#8:9]-[c:10]:[c:11](:[c:12])-[C;H0;D3;+0:13]-1=[O;H0;D1;+0:14]>>[C;D1;H3:6]-[C:7]1(-[C;D1;H3:8])-[#8:9]-[c:10]:[c:11](:[c:12])-[C;H0;D4;+0:13]-1(-[OH;D1;+0:14])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
65
[{"value": 65.0, "product": "NC=1C(=C(C2=C(C(C(O2)(C)C)(O)C2=CC=C(C=C2)C)C1C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 4-bromotoluene (2.73 g, 16.0 mmol) in THF (30 mL) was added dropwise a solution of n-butyllithium in hexane (1.60 M, 10.0 mL, 16.0 mmol) under argon atmosphere at −78° C., and the mixture was stirred at the same temperature for 30 minutes. Then, to the reaction solution was added dropwise a solution of...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ketone
Tertiary alcohol
c1ccc2c(c1)CCO2.c1ccccc1
c1ccccc1.c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
Br-
O.C1CCOC1
null
0.5
Cc1c(C)c2c(c(C)c1N)C(=O)C(C)(C)O2.Cc1ccc(Br)cc1>O.C1CCOC1>Cc1ccc(C2(O)c3c(C)c(N)c(C)c(C)c3OC2(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-10463635bd034e0bb913030ee8f322a7
CC(C)C(=O)c1ccc(C(C)C)cc1.COc1ccccc1Br>>COc1ccccc1C(O)(c1ccc(C(C)C)cc1)C(C)C
O.C(C)(C)C1=CC=C(C=C1)C(C(C)C)=O.BrC1=C(C=CC=C1)OC.C(CCC)[Li]>>C(C)(C)C1=CC=C(C=C1)C(C(C)C)(O)C1=C(C=CC=C1)OC
[C:9](=[O:10])([c:11]1[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]1)[CH:20]([CH3:21])[CH3:22].Br[c:8]1[c:3]([O:2][CH3:1])[cH:4][cH:5][cH:6][cH:7]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][cH:7][c:8]1[C:9]([OH:10])([c:11]1[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]1)[CH:20]([CH3:21])[CH3:...
CC(C)C(=O)c1ccc(C(C)C)cc1.COc1ccccc1Br
COc1ccccc1C(O)(c1ccc(C(C)C)cc1)C(C)C
null
null
C1CCOC1
C-C Coupling
Grignard_alcohol
23831eb2f5100c758a065f977b2daac4728a2009a2a7f37e9b01c50283e9e583
b8801be51258f6ee39fb6aad45dd9677b1b9eed3d6e0018ffb065bca8e787abf
c1ccc(Cc2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4](-[#8:5]):[c:6].[C;D1;H3:7]-[C:8](-[C;D1;H3:9])-[C;H0;D3;+0:10](=[O;H0;D1;+0:11])-[c:12](:[c:13]):[c:14]>>[#8:5]-[c:4](:[c:6]):[c;H0;D3;+0:1](-[C;H0;D4;+0:10](-[OH;D1;+0:11])(-[C:8](-[C;D1;H3:7])-[C;D1;H3:9])-[c:12](:[c:13]):[c:14]):[c:2]:[c:3]
43
[{"value": 43.0, "product": "C(C)(C)C1=CC=C(C=C1)C(C(C)C)(O)C1=C(C=CC=C1)OC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 42.7, "product": "C(C)(C)C1=CC=C(C=C1)C(C(C)C)(O)C1=C(C=CC=C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 2-bromoanisole (5.0 g, 26.7 mmol) in THF (50 mL) was added n-butyllithium (1.6 M, 18 mL, 29 mmol) at −78° C., and the mixture was stirred at the same temperature for 30 minutes. To the reaction solution was added 1-(4-isopropylphenyl)-2-methylpropan-1-one (5.70 g, 30.0 mmol), and the mixture was stirre...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Ketone
Tertiary alcohol
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
Br-
C1CCOC1
null
0.5
CC(C)C(=O)c1ccc(C(C)C)cc1.COc1ccccc1Br>C1CCOC1>COc1ccccc1C(O)(c1ccc(C(C)C)cc1)C(C)C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-7bd353d044cb4991b15f00dce48178be
COc1ccccc1C(O)(c1ccc(C(C)C)cc1)C(C)C>>CC(C)c1ccc(C2c3ccccc3OC2(C)C)cc1
C(C)(=O)O.C(C)(C)C1=CC=C(C=C1)C(C(C)C)(O)C1=C(C=CC=C1)OC.O.Br>>C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C=CC=C2)(C)C
C[O:15][c:14]1[c:9]([C:8](O)([c:7]2[cH:6][cH:5][c:4]([CH:2]([CH3:1])[CH3:3])[cH:20][cH:19]2)[CH:16]([CH3:17])[CH3:18])[cH:10][cH:11][cH:12][cH:13]1>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH:8]2[c:9]3[cH:10][cH:11][cH:12][cH:13][c:14]3[O:15][C:16]2([CH3:17])[CH3:18])[cH:19][cH:20]1
COc1ccccc1C(O)(c1ccc(C(C)C)cc1)C(C)C
CC(C)c1ccc(C2c3ccccc3OC2(C)C)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
58c1e8a6b0fb54736fce12602887392a72c98dcd612152b5c542155d025eacf0
ba55b0723234e68b590be0c71b7a395362712495d20a4ad5682afa361fa48a3a
c1ccc(C2COc3ccccc32)cc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](-[C;H0;D4;+0:5](-O)(-[CH;D3;+0:6](-[C;D1;H3:7])-[C;D1;H3:8])-[c:9](:[c:10]):[c:11]):[c:12]>>[C;D1;H3:7]-[C;H0;D4;+0:6]1(-[C;D1;H3:8])-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4](:[c:12])-[CH;D3;+0:5]-1-[c:9](:[c:10]):[c:11]
89
[{"value": 89.0, "product": "C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C=CC=C2)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixture of 1-(4-isopropylphenyl)-1-(2-methoxyphenyl)-2-methylpropan-1-ol obtained in Reference Example 82 (3.4 g, 11.4 mmol), 48% hydrobromic acid (50 mL) and acetic acid (10 mL) was heated under reflux under argon atmosphere for 16 hours. After cooling, water was added to the reaction solution, which was extracted w...
10.6084/m9.figshare.5104873.v1
null
Ether.Tertiary alcohol
Ether
null
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
HO-
null
null
null
COc1ccccc1C(O)(c1ccc(C(C)C)cc1)C(C)C>>CC(C)c1ccc(C2c3ccccc3OC2(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fc28da186ba54fde928140f29e5b9422
CC(C)c1ccc(C2c3cc(NCc4ccccc4)ccc3OC2(C)C)cc1>>CC(C)c1ccc(C2c3cc(N)ccc3OC2(C)C)cc1
C(C1=CC=CC=C1)NC=1C=CC2=C(C(C(O2)(C)C)C2=CC=C(C=C2)C(C)C)C1>>C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C=C(C=C2)N)(C)C
c1ccc(C[NH:12][c:11]2[cH:10][c:9]3[c:15]([cH:14][cH:13]2)[O:16][C:17]([CH3:18])([CH3:19])[CH:8]3[c:7]2[cH:6][cH:5][c:4]([CH:2]([CH3:1])[CH3:3])[cH:21][cH:20]2)cc1>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([CH:8]2[c:9]3[cH:10][c:11]([NH2:12])[cH:13][cH:14][c:15]3[O:16][C:17]2([CH3:18])[CH3:19])[cH:20][cH:21]1
CC(C)c1ccc(C2c3cc(NCc4ccccc4)ccc3OC2(C)C)cc1
CC(C)c1ccc(C2c3cc(N)ccc3OC2(C)C)cc1
null
null
CCCCCC
Deprotection
OtherReaction
93c46c2f9981b731115295839d7158a8a73faedd00707b7604ace2fa5f580cbc
f6571fb5b7780a2b467937abfba91ba7d787f19d503265f299ff4a25a08963bd
c1ccc(C2COc3ccccc32)cc1
[c:1]:[c:2](-[NH;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]>>[NH2;D1;+0:3]-[c:2](:[c:1]):[c:4]
98
[{"value": 98.0, "product": "C(C)(C)C1=CC=C(C=C1)C1C(OC2=C1C=C(C=C2)N)(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using N-benzyl-3-(4-isopropylphenyl)-2,2-dimethyl-2,3-dihydro-1-benzofuran-5-amine obtained in Reference Example 85, the title compound was synthesized in the same manner as in Reference Example 30. Yield 98%. Melting point: 109-110° C. (hexane). Conditions: See reaction.notes.procedure_details. Workup: obtained in Ref...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Primary amine
c1ccccc1
null
c1ccccc1.c1ccc2c(c1)CCO2
Other
CCCCCC
null
null
CC(C)c1ccc(C2c3cc(NCc4ccccc4)ccc3OC2(C)C)cc1>CCCCCC>CC(C)c1ccc(C2c3cc(N)ccc3OC2(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-aad60748f30349b1b484680a1b3b7c84
CC(=Cc1ccc(C(C)C)cc1)CBr.Cc1ccc(O)cc1>>CC(=Cc1ccc(C(C)C)cc1)COc1ccc(C)cc1
O.BrCC(=CC1=CC=C(C=C1)C(C)C)C.C1=CC(=CC=C1O)C.[H-].[Na+]>>C(C)(C)C1=CC=C(C=C1)C=C(COC1=CC=C(C=C1)C)C
Br[CH2:13][C:2]([CH3:1])=[CH:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH3:9])[CH3:10])[cH:11][cH:12]1.[OH:14][c:15]1[cH:16][cH:17][c:18]([CH3:19])[cH:20][cH:21]1>>[CH3:1][C:2](=[CH:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH3:9])[CH3:10])[cH:11][cH:12]1)[CH2:13][O:14][c:15]1[cH:16][cH:17][c:18]([CH3:19])[cH:20][cH:21]1
CC(=Cc1ccc(C(C)C)cc1)CBr.Cc1ccc(O)cc1
CC(=Cc1ccc(C(C)C)cc1)COc1ccc(C)cc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
C(=Cc1ccccc1)COc1ccccc1
Br-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])=[C:4]-[c:5].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[C;D1;H3:3]-[C:2](=[C:4]-[c:5])-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]
91
[{"value": 91.0, "product": "C(C)(C)C1=CC=C(C=C1)C=C(COC1=CC=C(C=C1)C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 90.5, "product": "C(C)(C)C1=CC=C(C=C1)C=C(COC1=CC=C(C=C1)C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of p-cresol (3.50 g, 32.3 mmol) in DMF (70 mL) was added sodium hydride (a 60% liquid paraffin dispersion, 1.42 g, 35.5 mmol) under nitrogen atmosphere at 0° C., and the mixture was stirred at the same temperature for 30 minutes. To the reaction solution was added 1-(3-bromo-2-methyl-1-propenyl)-4-isoprop...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccccc1
HBr
CN(C)C=O
null
0.5
CC(=Cc1ccc(C(C)C)cc1)CBr.Cc1ccc(O)cc1>CN(C)C=O>CC(=Cc1ccc(C(C)C)cc1)COc1ccc(C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d38422b333b540758dabc5502807840a
CC(=Cc1ccc(C(C)C)cc1)COc1ccc(C)cc1>>C=C(C)C(c1ccc(C(C)C)cc1)c1cc(C)ccc1O
C(C)(C)C1=CC=C(C=C1)C=C(COC1=CC=C(C=C1)C)C>>C(C)(C)C1=CC=C(C=C1)C(C(=C)C)C1=C(C=CC(=C1)C)O
[CH2:1]([C:2]([CH3:3])=[CH:4][c:5]1[cH:6][cH:7][c:8]([CH:9]([CH3:10])[CH3:11])[cH:12][cH:13]1)[O:21][c:20]1[cH:14][cH:15][c:16]([CH3:17])[cH:18][cH:19]1>>[CH2:1]=[C:2]([CH3:3])[CH:4]([c:5]1[cH:6][cH:7][c:8]([CH:9]([CH3:10])[CH3:11])[cH:12][cH:13]1)[c:14]1[cH:15][c:16]([CH3:17])[cH:18][cH:19][c:20]1[OH:21]
CC(=Cc1ccc(C(C)C)cc1)COc1ccc(C)cc1
C=C(C)C(c1ccc(C(C)C)cc1)c1cc(C)ccc1O
null
null
CN(C1=CC=CC=C1)C.C(C)(C)OC(C)C
Miscellaneous
OtherReaction
b75155b152f2323e33b77ed6ec85548ee0adafb0a5b89b0b2df41caeacf0b82c
39a337f27c7b73d892a2a429733dfdd8800f0f2eed92269e198b5632100ca547
c1ccc(Cc2ccccc2)cc1
[C;D1;H3:1]-[C;H0;D3;+0:2](-[CH2;D2;+0:3]-[O;H0;D2;+0:4]-[c:5](:[c:6]):[cH;D2;+0:7]:[c:8]:[c:9])=[CH;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[C;D1;H3:1]-[C;H0;D3;+0:2](=[CH2;D1;+0:3])-[CH;D3;+0:10](-[c:11](:[c:12]):[c:13])-[c;H0;D3;+0:7](:[c:8]:[c:9]):[c:5](-[OH;D1;+0:4]):[c:6]
95
[{"value": 95.0, "product": "C(C)(C)C1=CC=C(C=C1)C(C(=C)C)C1=C(C=CC(=C1)C)O", "details": "PERCENTYIELD", "is_desired": false}]
215
CELSIUS
16
HOUR
A solution of 1-isopropyl-4-(2-methyl-3-(4-methylphenoxy)propene-1-yl)benzene obtained in Reference Example 87 (8.2 g, 29.2 mmol) in N,N-dimethylaniline (50 mL) was stirred under argon atmosphere at 215° C. for 16 hours. After cooling, the reaction mixture was diluted with diisopropyl ether, washed with 5 N hydrochlori...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol.Vinyl
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
null
CN(C1=CC=CC=C1)C.C(C)(C)OC(C)C
215
16
CC(=Cc1ccc(C(C)C)cc1)COc1ccc(C)cc1>CN(C1=CC=CC=C1)C.C(C)(C)OC(C)C>C=C(C)C(c1ccc(C(C)C)cc1)c1cc(C)ccc1O
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-67ca99a570af446a9db2b4ad41adf7bc
Cc1cc2c(c(C)c1NCc1ccccc1)C(=O)C(C)(C)O2>>Cc1cc2c(c(C)c1NCc1ccccc1)C(O)C(C)(C)O2
C(C1=CC=CC=C1)NC=1C(=CC2=C(C(C(O2)(C)C)=O)C1C)C.[BH4-].[Na+]>>C(C1=CC=CC=C1)NC=1C(=CC2=C(C(C(O2)(C)C)O)C1C)C
[CH3:1][c:2]1[cH:3][c:4]2[c:5]([c:6]([CH3:7])[c:8]1[NH:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[C:17](=[O:18])[C:19]([CH3:20])([CH3:21])[O:22]2>>[CH3:1][c:2]1[cH:3][c:4]2[c:5]([c:6]([CH3:7])[c:8]1[NH:9][CH2:10][c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[CH:17]([OH:18])[C:19]([CH3:20])([CH3:21])[O:22]2
Cc1cc2c(c(C)c1NCc1ccccc1)C(=O)C(C)(C)O2
Cc1cc2c(c(C)c1NCc1ccccc1)C(O)C(C)(C)O2
null
null
CO
Reduction
Reduction of ketone to secondary alcohol
755c7bdda3ccaa9e2a097b82c386f43f2881f1d49e6c3707dce72c3ac00b51db
1bd3cd74b454139c0a0068ac0135836499926b274bff569df163210c6c944a89
c1ccc(CNc2ccc3c(c2)CCO3)cc1
[C;D1;H3:1]-[C:2]1(-[C;D1;H3:3])-[#8:4]-[c:5]:[c:6](:[c:7])-[C;H0;D3;+0:8]-1=[O;H0;D1;+0:9]>>[C;D1;H3:1]-[C:2]1(-[C;D1;H3:3])-[#8:4]-[c:5]:[c:6](:[c:7])-[CH;D3;+0:8]-1-[OH;D1;+0:9]
null
[]
null
null
2
HOUR
To a solution of 5-(benzylamino)-2,2,4,6-tetramethyl-1-benzofuran-3(2H)-one obtained in Reference Example 51 (8.5 g, 28.8 mmol) in methanol (20 mL) was added sodium borohydride (2.18 g, 57.6 mmol) at room temperature, and the mixture was stirred for 2 hours. The reaction solution was concentrated under reduced pressure...
10.6084/m9.figshare.5104873.v1
null
Ketone
Secondary alcohol
c1ccc2c(c1)CCO2
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
null
CO
null
2
Cc1cc2c(c(C)c1NCc1ccccc1)C(=O)C(C)(C)O2>CO>Cc1cc2c(c(C)c1NCc1ccccc1)C(O)C(C)(C)O2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-7399efa988b74eafa43d6ae871129c0d
CC(C)c1ccc(C=O)cc1.CCOC(=O)C(C)P(=O)(OCC)OCC>>CCOC(=O)C(C)=Cc1ccc(C(C)C)cc1
CCOC(=O)C(C)P(=O)(OCC)OCC.O.[H-].[Na+].C(C)(C)C1=CC=C(C=O)C=C1>>C(C)(C)C1=CC=C(C=C1)C=C(C(=O)OCC)C
O=[CH:8][c:9]1[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][cH:17]1.CCOP(=O)(OCC)[CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH3:7]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])=[CH:8][c:9]1[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][cH:17]1
CC(C)c1ccc(C=O)cc1.CCOC(=O)C(C)P(=O)(OCC)OCC
CCOC(=O)C(C)=Cc1ccc(C(C)C)cc1
null
null
CN(C)C=O
C-C Coupling
OtherReaction
a86984aeb4a9963534e0b081b0ecca18455fda1775f36ce168d1ca4cf966df3e
203dd34a20dceaf1737adbf20e01b43c2424e4e4b1722d942d1a796d895396e6
c1ccccc1
C-C-O-P(=O)(-O-C-C)-[CH;D3;+0:1](-[C;D1;H3:2])-[C:3](=[O;D1;H0:4])-[#8:5]-[C:6].O=[CH;D2;+0:7]-[c:8](:[c:9]):[c:10]>>[C:6]-[#8:5]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:1](-[C;D1;H3:2])=[CH;D2;+0:7]-[c:8](:[c:9]):[c:10]
96
[{"value": 96.0, "product": "C(C)(C)C1=CC=C(C=C1)C=C(C(=O)OCC)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 96.0, "product": "C(C)(C)C1=CC=C(C=C1)C=C(C(=O)OCC)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a suspension of sodium hydride (a 60% liquid paraffin dispersion, 5.92 g, 148 mmol) in DMF (150 mL) was added triethyl 2-phosphonopropionate (35.0 g, 148 mmol) at 0° C., and the mixture was stirred at the same temperature for 10 minutes. To the reaction solution was added 4-isopropylbenzaldehyde (20.0 g, 135 mmol), ...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ester
Ester
null
null
c1ccccc1
HO-
CN(C)C=O
null
0.166667
CC(C)c1ccc(C=O)cc1.CCOC(=O)C(C)P(=O)(OCC)OCC>CN(C)C=O>CCOC(=O)C(C)=Cc1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-01e411290f4348ac86830b8e10f70f16
CC(C)(C)[O-].O=Cc1ccc(Br)cc1>>CC(=Cc1ccc(Br)cc1)CO
O.BrC1=CC=C(C=O)C=C1.CC(C)([O-])C.[Na+]>>BrC1=CC=C(C=C1)C=C(CO)C
C[C:2]([O-])([CH3:1])[CH3:11].[CH:3]([c:4]1[cH:5][cH:6][c:7]([Br:8])[cH:9][cH:10]1)=[O:12]>>[CH3:1][C:2](=[CH:3][c:4]1[cH:5][cH:6][c:7]([Br:8])[cH:9][cH:10]1)[CH2:11][OH:12]
CC(C)(C)[O-].O=Cc1ccc(Br)cc1
CC(=Cc1ccc(Br)cc1)CO
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
f11de8ce6aae1931b2743d1c37dcfa7e7c31545d382a6d6f5c37348a82cd84f9
4f4da0c1ebb77155de3f9ccc4c0dc6683bc5c9f8cb0ed7c893695027b0c499da
c1ccccc1
C-[C;H0;D4;+0:1](-[C;D1;H3:2])(-[CH3;D1;+0:3])-[O-].[O;H0;D1;+0:4]=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8]>>[C;D1;H3:2]-[C;H0;D3;+0:1](-[CH2;D2;+0:3]-[OH;D1;+0:4])=[CH;D2;+0:5]-[c:6](:[c:7]):[c:8]
88
[{"value": 88.0, "product": "BrC1=CC=C(C=C1)C=C(CO)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of sodium tert-butoxide (10.6 g, 110 mmol) in DMF (60 mL) was added triethyl phosphonoacetate (26.2 g, 110 mmol) under argon atmosphere at −10° C. and the mixture was stirred at the same temperature for 1 hour. 4-bromobenzaldehyde (18.5 g, 100 mmol) was added to the solution at 10° C. or lower, and the mi...
10.6084/m9.figshare.5104873.v1
null
Aldehyde
Primary alcohol
null
null
c1ccccc1
HO-
CN(C)C=O
null
1
CC(C)(C)[O-].O=Cc1ccc(Br)cc1>CN(C)C=O>CC(=Cc1ccc(Br)cc1)CO
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-6e20631283514e81b42c54b67862b580
BrP(Br)Br.CC(=Cc1ccc(C(C)C)cc1)CO>>CC(=Cc1ccc(C(C)C)cc1)CBr
O.C(C)(C)C1=CC=C(C=C1)C=C(CO)C.P(Br)(Br)Br>>BrCC(=CC1=CC=C(C=C1)C(C)C)C
BrP(Br)[Br:14].O[CH2:13][C:2]([CH3:1])=[CH:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH3:9])[CH3:10])[cH:11][cH:12]1>>[CH3:1][C:2](=[CH:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH3:9])[CH3:10])[cH:11][cH:12]1)[CH2:13][Br:14]
BrP(Br)Br.CC(=Cc1ccc(C(C)C)cc1)CO
CC(=Cc1ccc(C(C)C)cc1)CBr
null
null
C(C)(C)OC(C)C
Functional Group Interconversion
PBr3 and alcohol to alkyl bromide
bb752b9027dc4488ba075e5955118a819f80cabd751a7497b67c2eeb1db6b071
cbf41c7cf9fe6b47a243b1674d74ed5bf46a151f7f3a71d206e23176e158facf
c1ccccc1
Br-P(-Br)-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3](-[C;D1;H3:4])=[C:5]-[c:6]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](-[C;D1;H3:4])=[C:5]-[c:6]
91
[{"value": 91.0, "product": "BrCC(=CC1=CC=C(C=C1)C(C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 3-(4-isopropylphenyl)-2-methyl-2-propen-1-ol synthesized in Reference Example 103 (6.30 g, 33.1 mmol) in isopropyl ether (50 mL) was added phosphorus tribromide (5.98 g, 22.1 mmol) with ice-cooling and the mixture was stirred at room temperature for 30 minutes. Water was added to the reaction solution ...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Primary halide
null
null
c1ccccc1
HBr
C(C)(C)OC(C)C
null
0.5
BrP(Br)Br.CC(=Cc1ccc(C(C)C)cc1)CO>C(C)(C)OC(C)C>CC(=Cc1ccc(C(C)C)cc1)CBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-cc294752030e42309020e2ebf11e0a9f
BrBr.CC(=Cc1ccc(Br)cc1)CO>>CC(=Cc1ccc(Br)cc1)CBr
BrC1=CC=C(C=C1)C=C(CO)C.C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.BrBr>>BrC1=CC=C(C=C1)C=C(CBr)C
Br[Br:12].O[CH2:11][C:2]([CH3:1])=[CH:3][c:4]1[cH:5][cH:6][c:7]([Br:8])[cH:9][cH:10]1>>[CH3:1][C:2](=[CH:3][c:4]1[cH:5][cH:6][c:7]([Br:8])[cH:9][cH:10]1)[CH2:11][Br:12]
BrBr.CC(=Cc1ccc(Br)cc1)CO
CC(=Cc1ccc(Br)cc1)CBr
null
null
C(C)#N
Functional Group Interconversion
OtherReaction
bb752b9027dc4488ba075e5955118a819f80cabd751a7497b67c2eeb1db6b071
cbf41c7cf9fe6b47a243b1674d74ed5bf46a151f7f3a71d206e23176e158facf
c1ccccc1
Br-[Br;H0;D1;+0:1].O-[CH2;D2;+0:2]-[C:3](-[C;D1;H3:4])=[C:5]-[c:6]>>[Br;H0;D1;+0:1]-[CH2;D2;+0:2]-[C:3](-[C;D1;H3:4])=[C:5]-[c:6]
98
[{"value": 98.0, "product": "BrC1=CC=C(C=C1)C=C(CBr)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To an acetonitrile solution (180 mL) of triphenylphosphine (24.3 g, 92.7 mmol) was added dropwise bromine (4.78 mL, 185 mmol) at 0° C. and the mixture was stirred at the same temperature for 30 minutes. To the solution was added the acetonitrile solution (60 mL) of 3-(4-bromophenyl)-2-methyl-2-propen-1-ol obtained in R...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Primary halide
null
null
c1ccccc1
HBr
C(C)#N
null
0.5
BrBr.CC(=Cc1ccc(Br)cc1)CO>C(C)#N>CC(=Cc1ccc(Br)cc1)CBr
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-fc93ca00e0ac440ea16e69be383eabfa
CC(=Cc1ccc(C(C)C)cc1)CBr.Cc1cc(O)c(C)c(C)c1NC=O>>CC(=Cc1ccc(C(C)C)cc1)COc1cc(C)c(NC=O)c(C)c1C
O.OC1=C(C(=C(C(=C1)C)NC=O)C)C.[H-].[Na+].BrCC(=CC1=CC=C(C=C1)C(C)C)C>>C(C)(C)C1=CC=C(C=C1)C=C(COC1=C(C(=C(C(=C1)C)NC=O)C)C)C
Br[CH2:13][C:2]([CH3:1])=[CH:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH3:9])[CH3:10])[cH:11][cH:12]1.[OH:14][c:15]1[cH:16][c:17]([CH3:18])[c:19]([NH:20][CH:21]=[O:22])[c:23]([CH3:24])[c:25]1[CH3:26]>>[CH3:1][C:2](=[CH:3][c:4]1[cH:5][cH:6][c:7]([CH:8]([CH3:9])[CH3:10])[cH:11][cH:12]1)[CH2:13][O:14][c:15]1[cH:16][c:17]([CH3:18...
CC(=Cc1ccc(C(C)C)cc1)CBr.Cc1cc(O)c(C)c(C)c1NC=O
CC(=Cc1ccc(C(C)C)cc1)COc1cc(C)c(NC=O)c(C)c1C
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
7e1040116e3a4cf0e8ec5cc7865388d9cd0efabce6d320a1c25a36e411018d8b
d5f4610d46ccc0478471c5bc0fb862644eaf764bbc5d93badb39d54f6ec8e0a5
C(=Cc1ccccc1)COc1ccccc1
Br-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])=[C:4]-[c:5].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[C;D1;H3:3]-[C:2](=[C:4]-[c:5])-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]
63
[{"value": 63.0, "product": "C(C)(C)C1=CC=C(C=C1)C=C(COC1=C(C(=C(C(=C1)C)NC=O)C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
10
MINUTE
To a solution of N-(4-hydroxy-2,3,6-trimethylphenyl)formamide (3.00 g, 16.7 mmol) in DMF (30 mL) was added sodium hydride (a 60% liquid paraffin dispersion, 0.74 g, 18.4 mmol) under nitrogen atmosphere at 0° C., and the mixture was stirred at the same temperature for 10 minutes. To the reaction solution was added 1-(3-...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Aromatic alcohol
Ether
null
null
c1ccccc1.c1ccccc1
HBr
CN(C)C=O
null
0.166667
CC(=Cc1ccc(C(C)C)cc1)CBr.Cc1cc(O)c(C)c(C)c1NC=O>CN(C)C=O>CC(=Cc1ccc(C(C)C)cc1)COc1cc(C)c(NC=O)c(C)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-d581bba9f39d4e5893fa9a5b878182ff
COS(=O)(=O)OC.Cc1cc(O)c(C)c(C)c1NC=O>>COc1cc(C)c(NC=O)c(C)c1C
OC1=C(C(=C(C(=C1)C)NC=O)C)C.S(=O)(=O)(OC)OC>>COC1=C(C(=C(C(=C1)C)NC=O)C)C
COS(=O)(=O)O[CH3:1].[OH:2][c:3]1[cH:4][c:5]([CH3:6])[c:7]([NH:8][CH:9]=[O:10])[c:11]([CH3:12])[c:13]1[CH3:14]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH3:6])[c:7]([NH:8][CH:9]=[O:10])[c:11]([CH3:12])[c:13]1[CH3:14]
COS(=O)(=O)OC.Cc1cc(O)c(C)c(C)c1NC=O
COc1cc(C)c(NC=O)c(C)c1C
null
null
[OH-].[K+].CO
Heteroatom Alkylation and Arylation
Methylation of OH with DMS
b8b041187bac58376aae824630608e7deb49a01db3d652291f8b379c10d4e434
0f0966e3597a58033417ecee71659f4d0c082f95d46b1e52c95541e6e4a59086
c1ccccc1
C-O-S(=O)(=O)-O-[CH3;D1;+0:1].[OH;D1;+0:2]-[c:3](:[c:4]):[c:5]>>[CH3;D1;+0:1]-[O;H0;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
null
null
null
null
N-(4-Hydroxy-2,3,6-trimethylphenyl)formamide (30.0 g, 167 mmol) was dissolved in a mixed solvent of 4 N potassium hydroxide aqueous solution (100 mL) and methanol (300 mL), and dimethyl sulfate (42.0 g, 334 mmol) was added to the solution at room temperature and the mixture was heated under reflux for 14 hours. After i...
10.6084/m9.figshare.5104873.v1
null
Aromatic alcohol
Ether
null
null
c1ccccc1
HO-
[OH-].[K+].CO
null
null
COS(=O)(=O)OC.Cc1cc(O)c(C)c(C)c1NC=O>[OH-].[K+].CO>COc1cc(C)c(NC=O)c(C)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-c37d4500c67b446e91009abab96e2a2c
BrBr.COc1cc(C)c(NC(=O)OC(C)(C)C)c(C)c1C>>COc1c(C)c(C)c(NC(=O)OC(C)(C)C)c(C)c1Br
BrBr.COC1=C(C(=C(C(=C1)C)NC(OC(C)(C)C)=O)C)C.O.C(C)(=O)[O-].[Na+]>>BrC=1C(=C(C(=C(C1OC)C)C)NC(OC(C)(C)C)=O)C
Br[Br:20].[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]([CH3:7])[c:8]([NH:9][C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[c:17]([CH3:18])[cH:19]1>>[CH3:1][O:2][c:3]1[c:4]([CH3:5])[c:6]([CH3:7])[c:8]([NH:9][C:10](=[O:11])[O:12][C:13]([CH3:14])([CH3:15])[CH3:16])[c:17]([CH3:18])[c:19]1[Br:20]
BrBr.COc1cc(C)c(NC(=O)OC(C)(C)C)c(C)c1C
COc1c(C)c(C)c(NC(=O)OC(C)(C)C)c(C)c1Br
null
null
C(C)(=O)O
Functional Group Interconversion
Bromination
f6effe61353895b318215d8bd9b6bb1105cafbf7be8c217d748df587260b32c3
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccccc1
Br-[Br;H0;D1;+0:1].[#8:2]-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6](-[C;D1;H3:7]):[c:8]>>[#8:2]-[c:3](:[c:4]):[c;H0;D3;+0:5](-[Br;H0;D1;+0:1]):[c:6](-[C;D1;H3:7]):[c:8]
91
[{"value": 91.0, "product": "BrC=1C(=C(C(=C(C1OC)C)C)NC(OC(C)(C)C)=O)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of tert-butyl 4-methoxy-2,3,6-trimethylphenylcarbamate synthesized in Reference Example 128 (12.7 g, 47.9 mmol) and sodium acetate (4.72 g, 57.5 mmol) in acetic acid (50 mL) was added bromine (8.42 g, 52.7 mmol) at room temperature and the mixture was stirred at the same temperature for 1 hour. Water (80 ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccccc1
c1ccccc1
c1ccccc1
HBr
C(C)(=O)O
null
1
BrBr.COc1cc(C)c(NC(=O)OC(C)(C)C)c(C)c1C>C(C)(=O)O>COc1c(C)c(C)c(NC(=O)OC(C)(C)C)c(C)c1Br
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3a05f66c400044a38de6e293bd21ea72
COc1c(C)c(C)c(NC(=O)OC(C)(C)C)c(C)c1Br.Cc1ccc(C(=O)C(C)C)cc1>>Cc1ccc(C2c3c(C)c(N)c(C)c(C)c3OC2(C)C)cc1
BrC=1C(=C(C(=C(C1OC)C)C)NC(OC(C)(C)C)=O)C.Br.C(CCC)[Li].CC(C(=O)C1=CC=C(C=C1)C)C.[OH-].[Na+].C1CCOC1>>CC1(OC2=C(C1C1=CC=C(C=C1)C)C(=C(C(=C2C)C)N)C)C
CC(C)(C)OC(=O)[NH:11][c:10]1[c:8]([CH3:9])[c:7](Br)[c:16]([O:17]C)[c:14]([CH3:15])[c:12]1[CH3:13].O=[C:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:22][cH:21]1)[CH:18]([CH3:19])[CH3:20]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]2[c:7]3[c:8]([CH3:9])[c:10]([NH2:11])[c:12]([CH3:13])[c:14]([CH3:15])[c:16]3[O:17][C:18]2([CH3:19])[CH...
COc1c(C)c(C)c(NC(=O)OC(C)(C)C)c(C)c1Br.Cc1ccc(C(=O)C(C)C)cc1
Cc1ccc(C2c3c(C)c(N)c(C)c(C)c3OC2(C)C)cc1
null
null
O
Heteroatom Alkylation and Arylation
OtherReaction
83a921042e81c7df82d28156d0ec8c578208dfaf866a836d1760d925ef450c4d
8e3de543a4256d430df17aaec49274e2668ccfd8c14a580ba7df511ae08ad10e
c1ccc(C2COc3ccccc32)cc1
Br-[c;H0;D3;+0:1]1:[c:2](-[O;H0;D2;+0:3]-C):[c:4]:[c:5]:[c:6](-[NH;D2;+0:7]-C(=O)-O-C(-C)(-C)-C):[c:8]:1-[C;D1;H3:9].O=[C;H0;D3;+0:10](-[CH;D3;+0:11](-[C;D1;H3:12])-[C;D1;H3:13])-[c:14](:[c:15]):[c:16]>>[C;D1;H3:12]-[C;H0;D4;+0:11]1(-[C;D1;H3:13])-[O;H0;D2;+0:3]-[c:2]2:[c:4]:[c:5]:[c:6](-[NH2;D1;+0:7]):[c:8](-[C;D1;H3:...
62
[{"value": 62.0, "product": "CC1(OC2=C(C1C1=CC=C(C=C1)C)C(=C(C(=C2C)C)N)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
20
MINUTE
To a solution of tert-butyl 3-bromo-4-methoxy-2,5,6-trimethylphenylcarbamate synthesized in Reference Example 129 (27.8 g, 80.8 mmol) in THF (150 mL) was added n-butyllithium (1.6 M, 110 mL, 176 mmol) hexane solution at −78° C. and the mixture was stirred at the same temperature for 20 minutes. 2-Methyl-1-(4-methylphen...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carbamic ester.Ketone.Ether.Ether.Boc
Ether.Primary amine
c1ccccc1
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
HBr
O
null
0.333333
COc1c(C)c(C)c(NC(=O)OC(C)(C)C)c(C)c1Br.Cc1ccc(C(=O)C(C)C)cc1>O>Cc1ccc(C2c3c(C)c(N)c(C)c(C)c3OC2(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-89feb5e31fa848e9b03e5b269edaf633
CC(C)(Br)C(=O)c1ccc(Br)cc1.Cc1cccc(O)c1C>>Cc1ccc(C(=O)C(C)(C)Oc2cccc(C)c2C)cc1
O.CC1=C(C=CC=C1C)O.C([O-])([O-])=O.[K+].[K+].BrC(C(=O)C1=CC=C(C=C1)Br)(C)C>>CC1=C(OC(C(=O)C2=CC=C(C=C2)C)(C)C)C=CC=C1C
Br[c:2]1[cH:3][cH:4][c:5]([C:6](=[O:7])[C:8](Br)([CH3:9])[CH3:10])[cH:20][cH:21]1.[OH:11][c:12]1[cH:13][cH:14][cH:15][c:16]([CH3:17])[c:18]1[CH3:19]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6](=[O:7])[C:8]([CH3:9])([CH3:10])[O:11][c:12]2[cH:13][cH:14][cH:15][c:16]([CH3:17])[c:18]2[CH3:19])[cH:20][cH:21]1
CC(C)(Br)C(=O)c1ccc(Br)cc1.Cc1cccc(O)c1C
Cc1ccc(C(=O)C(C)(C)Oc2cccc(C)c2C)cc1
null
null
CS(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
2b2b214b3256905650efd4b30d39719df81dcdc20143eeaaad86e37ab684292b
9d666779d213eb35efd66c7c5f2a93415132bdf22366a901eff054e84b5f3b5d
O=C(COc1ccccc1)c1ccccc1
Br-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4](-[C:5](=[O;D1;H0:6])-[C;H0;D4;+0:7](-Br)(-[C;D1;H3:8])-[C;D1;H3:9]):[c:10]:[c:11]:1.[OH;D1;+0:12]-[c:13](:[c:14]):[c:15]>>[C;D1;H3:8]-[C;H0;D4;+0:7](-[C;D1;H3:9])(-[O;H0;D2;+0:12]-[c:13](:[c:14]):[c:15])-[C:5](=[O;D1;H0:6])-[c:4]1:[c:3]:[c:2]:[c;H0;D3;+0:1](-[C;D1;H3:16]):[c:11]:[c:...
null
[]
35
CELSIUS
24
HOUR
To a mixture of 2,3-dimethylphenol (12.2 g, 100 mmol) and potassium carbonate (27.4 g, 200 mmol) in dimethylsulfoxide (138 mL) was added 2-bromo-1-(4-bromophenyl)-2-methylpropane-1-one (42.2 g, 175 mmol) at room temperature, and the mixture was warmed to 35° C. The mixture was stirred at the same temperature for 24 hou...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Tertiary halide.Ketone.Aromatic alcohol
Ketone.Ether
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
Br-
CS(=O)C
35
24
CC(C)(Br)C(=O)c1ccc(Br)cc1.Cc1cccc(O)c1C>CS(=O)C>Cc1ccc(C(=O)C(C)(C)Oc2cccc(C)c2C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3b9d43123ec34e4f93e9ad96c6fa974a
Cc1ccc(C(O)C(C)(C)Oc2cccc(C)c2C)cc1>>Cc1ccc(C2c3ccc(C)c(C)c3OC2(C)C)cc1
C(O)([O-])=O.[Na+].CC1=C(OC(C(O)C2=CC=C(C=C2)C)(C)C)C=CC=C1C.FC(S(=O)(=O)[O-])(F)F>>CC1(OC2=C(C1C1=CC=C(C=C1)C)C=CC(=C2C)C)C
O[CH:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:20][cH:19]1)[C:16]([O:15][c:14]1[cH:7][cH:8][cH:9][c:10]([CH3:11])[c:12]1[CH3:13])([CH3:17])[CH3:18]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]2[c:7]3[cH:8][cH:9][c:10]([CH3:11])[c:12]([CH3:13])[c:14]3[O:15][C:16]2([CH3:17])[CH3:18])[cH:19][cH:20]1
Cc1ccc(C(O)C(C)(C)Oc2cccc(C)c2C)cc1
Cc1ccc(C2c3ccc(C)c(C)c3OC2(C)C)cc1
null
null
C1(=CC=CC=C1)C
Functional Group Interconversion
OtherReaction
65fcbc560307aa9109a332daa2c2899a0eac338a1489b81f286ef8fc2d062531
f8118e7f3e1d7109575c0c77239dee8da98ec71a2b23460bcda2084274bdf7e7
c1ccc(C2COc3ccccc32)cc1
O-[CH;D3;+0:1](-[c:2](:[c:3]):[c:4])-[C:5](-[C;D1;H3:6])(-[C;D1;H3:7])-[#8:8]-[c:9](:[c:10]):[cH;D2;+0:11]:[c:12]:[c:13]>>[C;D1;H3:6]-[C:5]1(-[C;D1;H3:7])-[#8:8]-[c:9](:[c:10]):[c;H0;D3;+0:11](:[c:12]:[c:13])-[CH;D3;+0:1]-1-[c:2](:[c:3]):[c:4]
58
[{"value": 58.0, "product": "CC1(OC2=C(C1C1=CC=C(C=C1)C)C=CC(=C2C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
50
CELSIUS
30
MINUTE
To a solution of 2-(2,3-dimethylphenoxy)-2-methyl-1-(4-methylphenyl)propane-1-ol synthesized in Reference Example 135 (17.0 g, 60 mmol) in toluene (200 mL) was added trifluoromethanesulfonate (0.53 mL, 6 mmol) at 0° C., and the mixture was warmed to 50° C. The mixture was stirred at the same temperature for 30 minutes ...
10.6084/m9.figshare.5104873.v1
null
Secondary alcohol
null
c1ccccc1
c1ccc2c(c1)CCO2
c1ccccc1.c1ccc2c(c1)CCO2
HO-
C1(=CC=CC=C1)C
50
0.5
Cc1ccc(C(O)C(C)(C)Oc2cccc(C)c2C)cc1>C1(=CC=CC=C1)C>Cc1ccc(C2c3ccc(C)c(C)c3OC2(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a0458a279ef14249bba2f2f0c0239953
Cc1ccc(C2c3cc(NCc4ccccc4)c(C)c(C)c3OC2(C)C)cc1>>Cc1ccc(C2c3cc(N)c(C)c(C)c3OC2(C)C)cc1
Cl.C(C1=CC=CC=C1)NC=1C(=C(C2=C(C(C(O2)(C)C)C2=CC=C(C=C2)C)C1)C)C>>CC1(OC2=C(C1C1=CC=C(C=C1)C)C=C(C(=C2C)C)N)C
c1ccc(C[NH:10][c:9]2[cH:8][c:7]3[c:15]([c:13]([CH3:14])[c:11]2[CH3:12])[O:16][C:17]([CH3:18])([CH3:19])[CH:6]3[c:5]2[cH:4][cH:3][c:2]([CH3:1])[cH:21][cH:20]2)cc1>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([CH:6]2[c:7]3[cH:8][c:9]([NH2:10])[c:11]([CH3:12])[c:13]([CH3:14])[c:15]3[O:16][C:17]2([CH3:18])[CH3:19])[cH:20][cH:21]1
Cc1ccc(C2c3cc(NCc4ccccc4)c(C)c(C)c3OC2(C)C)cc1
Cc1ccc(C2c3cc(N)c(C)c(C)c3OC2(C)C)cc1
null
[C].[Pd]
C(C)O
Deprotection
OtherReaction
93c46c2f9981b731115295839d7158a8a73faedd00707b7604ace2fa5f580cbc
f6571fb5b7780a2b467937abfba91ba7d787f19d503265f299ff4a25a08963bd
c1ccc(C2COc3ccccc32)cc1
[c:1]:[c:2](-[NH;D2;+0:3]-C-c1:c:c:c:c:c:1):[c:4]>>[NH2;D1;+0:3]-[c:2](:[c:1]):[c:4]
88
[{"value": 88.0, "product": "CC1(OC2=C(C1C1=CC=C(C=C1)C)C=C(C(=C2C)C)N)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a solution of N-benzyl-2,2,6,7-tetramethyl-3-(4-methylphenyl)-2,3-dihydro-1-benzofuran-5-amine obtained in Reference Example 138 (6.60 g, 17.8 mmol) in ethanol (70 mL) was added 12 N hydrochloric acid (0.1 mL) and 10%-palladium carbon (hydrous 50%, 0.33 g), and the mixture was stirred under hydrogen condition of 5 a...
10.6084/m9.figshare.5104873.v1
null
Secondary amine
Primary amine
c1ccccc1
null
c1ccccc1.c1ccc2c(c1)CCO2
Other
[C].[Pd].C(C)O
null
2
Cc1ccc(C2c3cc(NCc4ccccc4)c(C)c(C)c3OC2(C)C)cc1>[C].[Pd].C(C)O>Cc1ccc(C2c3cc(N)c(C)c(C)c3OC2(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-20f2e46b71124d74bb5bae7fedc8f625
Cc1cc2c(c(C)c1N)C(c1ccc(C(C)C)cc1)CO2>>Cc1cc2c(c(C)c1N)[C@@H](c1ccc(C(C)C)cc1)CO2
C(C)(C)C1=CC=C(C=C1)C1COC2=C1C(=C(C(=C2)C)N)C>>C(C)(C)C1=CC=C(C=C1)[C@H]1COC2=C1C(=C(C(=C2)C)N)C
[CH3:1][c:2]1[cH:3][c:4]2[c:5]([c:6]([CH3:7])[c:8]1[NH2:9])[CH:10]([c:11]1[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]1)[CH2:20][O:21]2>>[CH3:1][c:2]1[cH:3][c:4]2[c:5]([c:6]([CH3:7])[c:8]1[NH2:9])[C@@H:10]([c:11]1[cH:12][cH:13][c:14]([CH:15]([CH3:16])[CH3:17])[cH:18][cH:19]1)[CH2:20][O:21]2
Cc1cc2c(c(C)c1N)C(c1ccc(C(C)C)cc1)CO2
Cc1cc2c(c(C)c1N)[C@@H](c1ccc(C(C)C)cc1)CO2
null
null
C(C)O
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc([C@H]2COc3ccccc32)cc1
null
34
[{"value": 34.0, "product": "C(C)(C)C1=CC=C(C=C1)[C@H]1COC2=C1C(=C(C(=C2)C)N)C", "details": "PERCENTYIELD", "is_desired": false}]
85
CELSIUS
null
null
A suspension of 3-(4-isopropylphenyl)-4,6-dimethyl-2,3-dihydro-1-benzofuran-5-amine obtained in Reference Example 32 (22.5 g, 80 mmol) and (2S, 3S)-(4′-methyl)-tartranilic acid (19.14 g, 80 mmol) in ethanol (480 mL) was heated at 85° C. for dissolution. The solution was cooled to 0° C. for 2 hours, and the precipitated...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ccc2c(c1)CCO2
null
C(C)O
85
null
Cc1cc2c(c(C)c1N)C(c1ccc(C(C)C)cc1)CO2>C(C)O>Cc1cc2c(c(C)c1N)[C@@H](c1ccc(C(C)C)cc1)CO2
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-bdfdb7fc84a14927a0d813fd6345543c
CC(C)c1ccccc1.O=C(Br)CBr>>CC(C)c1ccc(C(=O)CBr)cc1
C1(=CC=CC=C1)C(C)C.[Cl-].[Al+3].[Cl-].[Cl-].BrCC(=O)Br>>BrCC(=O)C1=CC=C(C=C1)C(C)C
[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:12][cH:13]1.Br[C:8](=[O:9])[CH2:10][Br:11]>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])[CH2:10][Br:11])[cH:12][cH:13]1
CC(C)c1ccccc1.O=C(Br)CBr
CC(C)c1ccc(C(=O)CBr)cc1
null
null
ClCCl
C-C Coupling
Friedel-Crafts acylation
55541449ad4f182ef3dc0497085b282b1dcb76e0fb5ed140dc4eab4973eacb28
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
c1ccccc1
Br-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[Br;D1;H0:4].[c:5]:[c:6]:[cH;D2;+0:7]:[c:8]:[c:9]>>[Br;D1;H0:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:7](:[c:6]:[c:5]):[c:8]:[c:9]
null
[]
null
null
2
HOUR
To a solution of cumene (27.8 mL, 200 mmol) and aluminum chloride (32.0 g, 240 mmol) in dichloromethane (300 mL) was added bromoacetylbromide (19.1 mL, 220 mmol) at −10° C., and the mixture was stirred at the same temperature for 2 hours. The reaction solution was poured into ice-cold water, and an organic layer was se...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
c1ccccc1
c1ccccc1
c1ccccc1
HBr
ClCCl
null
2
CC(C)c1ccccc1.O=C(Br)CBr>ClCCl>CC(C)c1ccc(C(=O)CBr)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-0766e6e31bb0458ba9c4188e7527571d
COc1ccc(CCC(=O)O)cc1.Cc1ccc(C2c3cc(N)c(C)c(C)c3OC2(C)C)cc1>>COc1ccc(CCC(=O)Nc2cc3c(c(C)c2C)OC(C)(C)C3c2ccc(C)cc2)cc1
CC1(OC2=C(C1C1=CC=C(C=C1)C)C=C(C(=C2C)C)N)C.COC1=CC=C(C=C1)CCC(=O)O>>COC1=CC=C(C=C1)CCC(=O)NC=1C(=C(C2=C(C(C(O2)(C)C)C2=CC=C(C=C2)C)C1)C)C
O[C:9]([CH2:8][CH2:7][c:6]1[cH:5][cH:4][c:3]([O:2][CH3:1])[cH:33][cH:32]1)=[O:10].[NH2:11][c:12]1[cH:13][c:14]2[c:15]([c:16]([CH3:17])[c:18]1[CH3:19])[O:20][C:21]([CH3:22])([CH3:23])[CH:24]2[c:25]1[cH:26][cH:27][c:28]([CH3:29])[cH:30][cH:31]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][CH2:8][C:9](=[O:10])[NH:11][c:12...
COc1ccc(CCC(=O)O)cc1.Cc1ccc(C2c3cc(N)c(C)c(C)c3OC2(C)C)cc1
COc1ccc(CCC(=O)Nc2cc3c(c(C)c2C)OC(C)(C)C3c2ccc(C)cc2)cc1
null
null
null
Acylation
Carboxylic acid with primary amine to amide
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(CCc1ccccc1)Nc1ccc2c(c1)C(c1ccccc1)CO2
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[NH2;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[c:7]):[c:8]
64
[{"value": 64.0, "product": "COC1=CC=C(C=C1)CCC(=O)NC=1C(=C(C2=C(C(C(O2)(C)C)C2=CC=C(C=C2)C)C1)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2,2,6,7-tetramethyl-3-(4-methylphenyl)-2,3-dihydro-1-benzofuran-5-amine obtained Reference Example 139 and 3-(4-methoxyphenyl)propionic acid, the title compound was obtained in the same manner as in Reference Example 359. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccccc1.c1ccc2c(c1)CCO2.c1ccccc1
HO-
null
null
null
COc1ccc(CCC(=O)O)cc1.Cc1ccc(C2c3cc(N)c(C)c(C)c3OC2(C)C)cc1>>COc1ccc(CCC(=O)Nc2cc3c(c(C)c2C)OC(C)(C)C3c2ccc(C)cc2)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a8ec02a46067491c9fcf32a61bc6e041
CC(C)c1ccc(Br)cc1.Cc1cc(C)c(C=O)c(O)c1>>Cc1cc(C)c(C(O)c2ccc(C(C)C)cc2)c(O)c1
OC1=C(C=O)C(=CC(=C1)C)C.BrC1=CC=C(C=C1)C(C)C.C(CCC)[Li].CCCCCC>>OC(C1=C(C=C(C=C1C)C)O)C1=CC=C(C=C1)C(C)C
Br[c:9]1[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][cH:17]1.[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH:7]=[O:8])[c:18]([OH:19])[cH:20]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH:7]([OH:8])[c:9]2[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][cH:17]2)[c:18]([OH:19])[cH:20]1
CC(C)c1ccc(Br)cc1.Cc1cc(C)c(C=O)c(O)c1
Cc1cc(C)c(C(O)c2ccc(C(C)C)cc2)c(O)c1
null
null
O.C1CCOC1
C-C Coupling
Grignard_alcohol
0c8bc0f755f4d9a2cfce93ae43a9a9a531fa8ad86ff120aed0a18ba03c84e4d7
1c0bd0afc1d5e370e3c8193faf738f03752295e40fa0eb99c756011e9a4be26b
c1ccc(Cc2ccccc2)cc1
Br-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5].[O;H0;D1;+0:6]=[CH;D2;+0:7]-[c:8](:[c:9]):[c:10]>>[OH;D1;+0:6]-[CH;D3;+0:7](-[c:8](:[c:9]):[c:10])-[c;H0;D3;+0:1](:[c:2]:[c:3]):[c:4]:[c:5]
91
[{"value": 91.0, "product": "OC(C1=C(C=C(C=C1C)C)O)C1=CC=C(C=C1)C(C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
30
MINUTE
To a solution of 1-bromo-4-isopropylbenzene (3.32 g, 16.7 mmol) in THF (30 mL) was added dropwise n-butyllithium (a 1.59 M hexane solution, 9.2 mL, 14.7 mmol) under argon atmosphere at −78° C. The reaction solution was stirred for 30 minutes, a solution of 2-hydroxy-4,6-dimethylbenzaldehyde obtained in Reference Exampl...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aldehyde
Secondary alcohol
c1ccccc1
c1ccccc1
c1ccccc1.c1ccccc1
Br-
O.C1CCOC1
null
0.5
CC(C)c1ccc(Br)cc1.Cc1cc(C)c(C=O)c(O)c1>O.C1CCOC1>Cc1cc(C)c(C(O)c2ccc(C(C)C)cc2)c(O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-3ee0d8a924914801b3fbf562509f919b
Cc1cc(C)cc(O)c1.O=C1CCC(=O)N1Br>>Cc1cc(C)c(Br)c(O)c1
CC=1C=C(C=C(C1)C)O.BrN1C(CCC1=O)=O>>BrC1=C(C=C(C=C1C)C)O
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[cH:6][c:8]([OH:9])[cH:10]1.O=C1CCC(=O)N1[Br:7]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([Br:7])[c:8]([OH:9])[cH:10]1
Cc1cc(C)cc(O)c1.O=C1CCC(=O)N1Br
Cc1cc(C)c(Br)c(O)c1
null
null
C(=S)=S
Functional Group Interconversion
Bromination
48c1dcf50945076da40bbd7976060ec1ea74b3478ef8c25d67664232b218095c
0e444576b73669992a4073cc3f7b10ed52cb9df09f9f8e4042e39e6a602aa390
c1ccccc1
O=C1-C-C-C(=O)-N-1-[Br;H0;D1;+0:1].[C;D1;H3:2]-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6](-[O;D1;H1:7]):[c:8]>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:5](:[c:3](-[C;D1;H3:2]):[c:4]):[c:6](-[O;D1;H1:7]):[c:8]
66
[{"value": 66.0, "product": "BrC1=C(C=C(C=C1C)C)O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 65.9, "product": "BrC1=C(C=C(C=C1C)C)O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 3,5-dimethylphenol (15.0 g, 123 mmol) in carbon disulfide (330 mL) was slowly added N-bromosuccinimide (21.9 g, 123 mmol) in several batches with ice-cooling, and the mixture was stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure, and the precipitated crystals ...
10.6084/m9.figshare.5104873.v1
null
Tertiary amide.Tertiary amide
Aromatic halide
c1ccccc1.C1CCNC1
c1ccccc1
c1ccccc1
HO-
C(=S)=S
null
1
Cc1cc(C)cc(O)c1.O=C1CCC(=O)N1Br>C(=S)=S>Cc1cc(C)c(Br)c(O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ba9b7965008946d2ab79928044140f6f
CCOC(=O)CBr.Cc1cc(C)c(C)c(O)c1>>CCOC(=O)COc1cc(C)cc(C)c1C
CC1=C(C=C(C=C1C)C)O.BrCC(=O)OCC>>CC1=C(OCC(=O)OCC)C=C(C=C1C)C
Br[CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5].[OH:7][c:8]1[cH:9][c:10]([CH3:11])[cH:12][c:13]([CH3:14])[c:15]1[CH3:16]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][O:7][c:8]1[cH:9][c:10]([CH3:11])[cH:12][c:13]([CH3:14])[c:15]1[CH3:16]
CCOC(=O)CBr.Cc1cc(C)c(C)c(O)c1
CCOC(=O)COc1cc(C)cc(C)c1C
null
null
null
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
50d675b335c583a6ce22e1164b27a78b18b9ca447d45137820c344bcb6369217
0865de4e1853c59ac25437e36fd18b03329566cb9eff4b4f0ce70d5714692fd3
c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5].[OH;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[C:5]-[#8:4]-[C:2](=[O;D1;H0:3])-[CH2;D2;+0:1]-[O;H0;D2;+0:6]-[c:7](:[c:8]):[c:9]
null
[]
null
null
null
null
Using 2,3,5-trimethylphenol and ethyl bromoacetate, the title compound was synthesized in the same manner as in Reference Example 153. Yield: quantitative. Oily matter. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Aromatic alcohol
Ester.Ether
null
null
c1ccccc1
HBr
null
null
null
CCOC(=O)CBr.Cc1cc(C)c(C)c(O)c1>>CCOC(=O)COc1cc(C)cc(C)c1C
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-72b487fe63864ee6a023f5c38c9ffc86
CCOC(=O)C(C)(C)Oc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1>>Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(OC(C)(C)C(=O)O)c1
C(C)(C)C1=CC=C(CC2=C(OC(C(=O)OCC)(C)C)C=C(C=C2C)C)C=C1.[OH-].[Na+].C1CCOC1.Cl>>C(C)(C)C1=CC=C(CC2=C(OC(C(=O)O)(C)C)C=C(C=C2C)C)C=C1
CC[O:24][C:22]([C:19]([O:18][c:17]1[c:6]([CH2:7][c:8]2[cH:9][cH:10][c:11]([CH:12]([CH3:13])[CH3:14])[cH:15][cH:16]2)[c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:25]1)([CH3:20])[CH3:21])=[O:23]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH2:7][c:8]2[cH:9][cH:10][c:11]([CH:12]([CH3:13])[CH3:14])[cH:15][cH:16]2)[c:17]([O:18][C:19]...
CCOC(=O)C(C)(C)Oc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1
Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(OC(C)(C)C(=O)O)c1
null
null
CO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(Cc2ccccc2)cc1
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]
91
[{"value": 91.0, "product": "C(C)(C)C1=CC=C(CC2=C(OC(C(=O)O)(C)C)C=C(C=C2C)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixed solution of ethyl 2-(2-(4-isopropylbenzyl)-3,5-dimethylphenoxy)-2-methylpropanoate obtained in Reference Example 153 (6.65 g, 18.1 mmol) and a 8 N aqueous sodium hydroxide solution (4.5 mL) in methanol (40 mL)-THF (20 mL) was stirred at room temperature for 16 hours. The reaction solution was acidified with hyd...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccccc1
Other
CO
null
null
CCOC(=O)C(C)(C)Oc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1>CO>Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(OC(C)(C)C(=O)O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-76f55b6ab6db4b9986f1d9db704a757d
CCOC(=O)COc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1>>Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(OCC(=O)O)c1
C(C)(C)C1=CC=C(CC2=C(OCC(=O)OCC)C=C(C=C2C)C)C=C1>>C(C)(C)C1=CC=C(CC2=C(OCC(=O)O)C=C(C=C2C)C)C=C1
CC[O:22][C:20]([CH2:19][O:18][c:17]1[c:6]([CH2:7][c:8]2[cH:9][cH:10][c:11]([CH:12]([CH3:13])[CH3:14])[cH:15][cH:16]2)[c:4]([CH3:5])[cH:3][c:2]([CH3:1])[cH:23]1)=[O:21]>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH2:7][c:8]2[cH:9][cH:10][c:11]([CH:12]([CH3:13])[CH3:14])[cH:15][cH:16]2)[c:17]([O:18][CH2:19][C:20](=[O:21])[...
CCOC(=O)COc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1
Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(OCC(=O)O)c1
null
null
C(C)(=O)OCC.CCCCCC
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(Cc2ccccc2)cc1
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]
75
[{"value": 75.0, "product": "C(C)(C)C1=CC=C(CC2=C(OCC(=O)O)C=C(C=C2C)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using ethyl (2-(4-isopropylbenzyl)-3,5-dimethylphenoxy)acetate obtained in Reference Example 154, the title compound was synthesized in the same manner as in Reference Example 156. Yield 75%. Melting point: 104-105° C. (ethyl acetate-hexane). Conditions: See reaction.notes.procedure_details. Workup: obtained in Referen...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccccc1
Other
C(C)(=O)OCC.CCCCCC
null
null
CCOC(=O)COc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1>C(C)(=O)OCC.CCCCCC>Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(OCC(=O)O)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-841553179ead41ae92fb9726a38fef87
CC(=O)CCl.Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(O)c1>>CC(=O)COc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1
C(C)(C)C1=CC=C(CC2=C(C=C(C=C2C)C)O)C=C1.[I-].[K+].C([O-])([O-])=O.[K+].[K+].ClCC(C)=O>>C(C)(C)C1=CC=C(CC2=C(OCC(=O)C)C=C(C=C2C)C)C=C1
Cl[CH2:4][C:2]([CH3:1])=[O:3].[OH:5][c:6]1[cH:7][c:8]([CH3:9])[cH:10][c:11]([CH3:12])[c:13]1[CH2:14][c:15]1[cH:16][cH:17][c:18]([CH:19]([CH3:20])[CH3:21])[cH:22][cH:23]1>>[CH3:1][C:2](=[O:3])[CH2:4][O:5][c:6]1[cH:7][c:8]([CH3:9])[cH:10][c:11]([CH3:12])[c:13]1[CH2:14][c:15]1[cH:16][cH:17][c:18]([CH:19]([CH3:20])[CH3:21]...
CC(=O)CCl.Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(O)c1
CC(=O)COc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1
null
null
O.CC(=O)C
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8060b8e1565497a5ddf79be1adfe74f552b31798797b8841753247b06bdd2051
8749b179916f131d393264a24309227dc6177f560726bed2d1f4567dc2ac63f5
c1ccc(Cc2ccccc2)cc1
Cl-[CH2;D2;+0:1]-[C:2](-[C;D1;H3:3])=[O;D1;H0:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[C;D1;H3:3]-[C:2](=[O;D1;H0:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
73
[{"value": 73.0, "product": "C(C)(C)C1=CC=C(CC2=C(OCC(=O)C)C=C(C=C2C)C)C=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A mixed solution of 2-(4-isopropylbenzyl)-3,5-dimethylphenol obtained in Reference Example 148 (1.0 g, 3.93 mmol), potassium carbonate (1.30 g, 9.44 mmol), chloroacetone (436 mg, 4.72 mmol) and potassium iodide (100 mg) in acetone (15 mL) was heated under reflux for 16 hours. Water was added to the reaction solution, w...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Aromatic alcohol
Ketone.Ether
null
null
c1ccccc1.c1ccccc1
HCl
O.CC(=O)C
null
null
CC(=O)CCl.Cc1cc(C)c(Cc2ccc(C(C)C)cc2)c(O)c1>O.CC(=O)C>CC(=O)COc1cc(C)cc(C)c1Cc1ccc(C(C)C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-76328dece4224a42ac6d78dfe615c46b
Cc1cc(C)c(C)c(O)c1.O=C(CBr)c1cccc(Br)c1>>Cc1cc(C)c(C)c(OCC(=O)c2cccc(Br)c2)c1
CC1=C(C=C(C=C1C)C)O.BrCC(=O)C1=CC(=CC=C1)Br>>BrC=1C=C(C=CC1)C(COC1=C(C(=CC(=C1)C)C)C)=O
[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH3:7])[c:8]([OH:9])[cH:20]1.Br[CH2:10][C:11](=[O:12])[c:13]1[cH:14][cH:15][cH:16][c:17]([Br:18])[cH:19]1>>[CH3:1][c:2]1[cH:3][c:4]([CH3:5])[c:6]([CH3:7])[c:8]([O:9][CH2:10][C:11](=[O:12])[c:13]2[cH:14][cH:15][cH:16][c:17]([Br:18])[cH:19]2)[cH:20]1
Cc1cc(C)c(C)c(O)c1.O=C(CBr)c1cccc(Br)c1
Cc1cc(C)c(C)c(OCC(=O)c2cccc(Br)c2)c1
null
null
null
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8060b8e1565497a5ddf79be1adfe74f552b31798797b8841753247b06bdd2051
8749b179916f131d393264a24309227dc6177f560726bed2d1f4567dc2ac63f5
O=C(COc1ccccc1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[O;D1;H0:3]=[C:2](-[c:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
52
[{"value": 52.0, "product": "BrC=1C=C(C=CC1)C(COC1=C(C(=CC(=C1)C)C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2,3,5-trimethylphenol and 2-bromo-1-(3-bromophenyl)ethanone, the title compound was synthesized in the same manner as in Reference Example 159. Yield 52%. Oily matter. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Aromatic alcohol
Ketone.Ether
null
null
c1ccccc1.c1ccccc1
HBr
null
null
null
Cc1cc(C)c(C)c(O)c1.O=C(CBr)c1cccc(Br)c1>>Cc1cc(C)c(C)c(OCC(=O)c2cccc(Br)c2)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-52a2b141826c4269b5abfd8e957dd276
COc1cccc(C(=O)CBr)c1.Cc1cc(C)c(C)c(O)c1>>COc1cccc(C(=O)COc2cc(C)cc(C)c2C)c1
CC1=C(C=C(C=C1C)C)O.BrCC(=O)C1=CC(=CC=C1)OC>>COC=1C=C(C=CC1)C(COC1=C(C(=CC(=C1)C)C)C)=O
Br[CH2:10][C:8]([c:7]1[cH:6][cH:5][cH:4][c:3]([O:2][CH3:1])[cH:21]1)=[O:9].[OH:11][c:12]1[cH:13][c:14]([CH3:15])[cH:16][c:17]([CH3:18])[c:19]1[CH3:20]>>[CH3:1][O:2][c:3]1[cH:4][cH:5][cH:6][c:7]([C:8](=[O:9])[CH2:10][O:11][c:12]2[cH:13][c:14]([CH3:15])[cH:16][c:17]([CH3:18])[c:19]2[CH3:20])[cH:21]1
COc1cccc(C(=O)CBr)c1.Cc1cc(C)c(C)c(O)c1
COc1cccc(C(=O)COc2cc(C)cc(C)c2C)c1
null
null
null
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8060b8e1565497a5ddf79be1adfe74f552b31798797b8841753247b06bdd2051
8749b179916f131d393264a24309227dc6177f560726bed2d1f4567dc2ac63f5
O=C(COc1ccccc1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[O;D1;H0:3]=[C:2](-[c:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
88
[{"value": 88.0, "product": "COC=1C=C(C=CC1)C(COC1=C(C(=CC(=C1)C)C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2,3,5-trimethylphenol and 2-bromo-1-(3-methoxyphenyl)ethanone, the title compound was synthesized in the same manner as in Reference Example 159. Yield 88%. Oily matter. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Aromatic alcohol
Ketone.Ether
null
null
c1ccccc1.c1ccccc1
HBr
null
null
null
COc1cccc(C(=O)CBr)c1.Cc1cc(C)c(C)c(O)c1>>COc1cccc(C(=O)COc2cc(C)cc(C)c2C)c1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-a8f8409b65894cb8876433e12a2fb0d2
Cc1cc(C)c(C)c(O)c1.Cc1ccc(C(=O)CBr)cc1>>Cc1ccc(C(=O)COc2cc(C)cc(C)c2C)cc1
CC1=C(C=C(C=C1C)C)O.BrCC(=O)C1=CC=C(C=C1)C>>CC1=CC=C(C=C1)C(COC1=C(C(=CC(=C1)C)C)C)=O
[OH:9][c:10]1[cH:11][c:12]([CH3:13])[cH:14][c:15]([CH3:16])[c:17]1[CH3:18].Br[CH2:8][C:6]([c:5]1[cH:4][cH:3][c:2]([CH3:1])[cH:20][cH:19]1)=[O:7]>>[CH3:1][c:2]1[cH:3][cH:4][c:5]([C:6](=[O:7])[CH2:8][O:9][c:10]2[cH:11][c:12]([CH3:13])[cH:14][c:15]([CH3:16])[c:17]2[CH3:18])[cH:19][cH:20]1
Cc1cc(C)c(C)c(O)c1.Cc1ccc(C(=O)CBr)cc1
Cc1ccc(C(=O)COc2cc(C)cc(C)c2C)cc1
null
null
CO
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8060b8e1565497a5ddf79be1adfe74f552b31798797b8841753247b06bdd2051
8749b179916f131d393264a24309227dc6177f560726bed2d1f4567dc2ac63f5
O=C(COc1ccccc1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[O;D1;H0:3]=[C:2](-[c:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
75
[{"value": 75.0, "product": "CC1=CC=C(C=C1)C(COC1=C(C(=CC(=C1)C)C)C)=O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2,3,5-trimethylphenol and 2-bromo-1-(4-methylphenyl)ethanone, the title compound was synthesized in the same manner as in Reference Example 159. Yield 75%. Melting point: 94-95° C. (methanol). Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Aromatic alcohol
Ketone.Ether
null
null
c1ccccc1.c1ccccc1
HBr
CO
null
null
Cc1cc(C)c(C)c(O)c1.Cc1ccc(C(=O)CBr)cc1>CO>Cc1ccc(C(=O)COc2cc(C)cc(C)c2C)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-ffa3335c06624450a23b11b09c0ba6bf
CC(C)c1ccccc1.O=C(Br)CBr>>CC(C)c1ccc(C(=O)CBr)cc1
C1(=CC=CC=C1)C(C)C.[Cl-].[Al+3].[Cl-].[Cl-].BrCC(=O)Br>>BrCC(=O)C1=CC=C(C=C1)C(C)C
[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][cH:7][cH:12][cH:13]1.Br[C:8](=[O:9])[CH2:10][Br:11]>>[CH3:1][CH:2]([CH3:3])[c:4]1[cH:5][cH:6][c:7]([C:8](=[O:9])[CH2:10][Br:11])[cH:12][cH:13]1
CC(C)c1ccccc1.O=C(Br)CBr
CC(C)c1ccc(C(=O)CBr)cc1
null
null
ClCCl
C-C Coupling
Friedel-Crafts acylation
55541449ad4f182ef3dc0497085b282b1dcb76e0fb5ed140dc4eab4973eacb28
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
c1ccccc1
Br-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[Br;D1;H0:4].[c:5]:[c:6]:[cH;D2;+0:7]:[c:8]:[c:9]>>[Br;D1;H0:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c;H0;D3;+0:7](:[c:6]:[c:5]):[c:8]:[c:9]
99.5
[{"value": 99.0, "product": "BrCC(=O)C1=CC=C(C=C1)C(C)C", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.5, "product": "BrCC(=O)C1=CC=C(C=C1)C(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
-10
CELSIUS
null
null
To a solution of cumene (42 g, 350 mmol) and aluminum chloride (56.0 g, 420 mmol) in dichloromethane (500 mL) was added bromoacetylbromide (33.5 mL, 385 mmol) at −40° C. for 40 minutes, and the mixture was stirred until it was warmed to −10° C. for 2 hours. The reaction solution was poured into ice-cold water to separa...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
c1ccccc1
c1ccccc1
c1ccccc1
HBr
ClCCl
-10
null
CC(C)c1ccccc1.O=C(Br)CBr>ClCCl>CC(C)c1ccc(C(=O)CBr)cc1
ord_dataset-c31cb9b44c404c10ba3aa533aa079e2b
ord-cf23ff1a360c478e808d10ef0f6751b0
CC(C)c1ccc(C(=O)CBr)cc1.Cc1cc(O)c(C)c(C)c1Br>>Cc1cc(OCC(=O)c2ccc(C(C)C)cc2)c(C)c(C)c1Br
CC1=C(C=C(C=C1C)C)O.BrC1=C(C(=C(C=C1C)O)C)C.BrCC(=O)C1=CC=C(C=C1)C(C)C>>BrC1=C(C(=C(OCC(=O)C2=CC=C(C=C2)C(C)C)C=C1C)C)C
Br[CH2:6][C:7](=[O:8])[c:9]1[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][cH:17]1.[CH3:1][c:2]1[cH:3][c:4]([OH:5])[c:18]([CH3:19])[c:20]([CH3:21])[c:22]1[Br:23]>>[CH3:1][c:2]1[cH:3][c:4]([O:5][CH2:6][C:7](=[O:8])[c:9]2[cH:10][cH:11][c:12]([CH:13]([CH3:14])[CH3:15])[cH:16][cH:17]2)[c:18]([CH3:19])[c:20]([CH3:21...
CC(C)c1ccc(C(=O)CBr)cc1.Cc1cc(O)c(C)c(C)c1Br
Cc1cc(OCC(=O)c2ccc(C(C)C)cc2)c(C)c(C)c1Br
null
null
C(C)(=O)OCC.CCCCCC
Heteroatom Alkylation and Arylation
Williamson Ether Synthesis
8060b8e1565497a5ddf79be1adfe74f552b31798797b8841753247b06bdd2051
8749b179916f131d393264a24309227dc6177f560726bed2d1f4567dc2ac63f5
O=C(COc1ccccc1)c1ccccc1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[c:4].[OH;D1;+0:5]-[c:6](:[c:7]):[c:8]>>[O;D1;H0:3]=[C:2](-[c:4])-[CH2;D2;+0:1]-[O;H0;D2;+0:5]-[c:6](:[c:7]):[c:8]
51
[{"value": 51.0, "product": "BrC1=C(C(=C(OCC(=O)C2=CC=C(C=C2)C(C)C)C=C1C)C)C", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using 2,3,5-trimethylphenol, 4-bromo-2,3,5-trimethylphenol was synthesized in the same manner as in Reference Example 23. Using this compound and 2-bromo-1-(4-isopropylphenyl)ethanone obtained in Reference Example 164, the title compound was synthesized in the same manner as in Reference Example 159. Yield 51%. Melting...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ketone.Aromatic alcohol
Ketone.Ether
null
null
c1ccccc1.c1ccccc1
HBr
C(C)(=O)OCC.CCCCCC
null
null
CC(C)c1ccc(C(=O)CBr)cc1.Cc1cc(O)c(C)c(C)c1Br>C(C)(=O)OCC.CCCCCC>Cc1cc(OCC(=O)c2ccc(C(C)C)cc2)c(C)c(C)c1Br