HRID1521461

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6342

Acetonitrile

C2H3N

HCID8857

Ethyl acetate

C4H8O2

HCID521998

4-Methylbenzenesulfonic acid hydrate

C7H10O4S

结构：Cn1ncc2c1Nc1cc(Cl)ccc1N(C(=O)c1ccc(CNC(=O)C3CC3)c(F)c1)C2

HCID135564707

未命名化合物

PRODUCTS

生成物

结构：Cc1ccc(S(=O)(=O)O)cc1.Cn1ncc2c1Nc1cc(Cl)ccc1N(C(=O)c1ccc(CNC(=O)C3CC3)c(F)c1)C2

HCID135565015

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6560

2-Methyl-1-propanol

C4H10O

溶剂HCID66787386

未命名化合物

PROCEDURE

实验过程

A solution of para-toluenesulfonic acid monohydrate in iso-butanol was added to a solution of cyclopropanecarboxylic acid 4-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraazabenzo[f]azulene-9-carbonyl)-2-fluoro-benzylamide in toluene/iso-butanol. Acetonitrile and ethyl acetate were added. The solution was allowed to cool and seeded with crystals of the title compound (as prepared herein above). After further cooling and stirring, the product was isolated by filtration, washed with ethyl acetate and then dried.

WORKUP

后处理

temperatureto cool

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-ed5fde46edf04fd1932b7de1cb17a256
来源数据集: uspto-grants-2015_07
DOI: 10.6084/m9.figshare.5104873.v1
专利: US09073928B2
来源说明: uspto-grants-2015_07

反应 SMILES

O.[C:2]1([CH3:12])[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[Cl:13][C:14]1[CH:15]=[CH:16][C:17]2[N:26]([C:27]([C:29]3[CH:41]=[CH:40][C:32]([CH2:33][NH:34][C:35]([CH:37]4[CH2:39][CH2:38]4)=[O:36])=[C:31]([F:42])[CH:30]=3)=[O:28])[CH2:25][C:24]3[CH:23]=[N:22][N:21]([CH3:43])[C:20]=3[NH:19][C:18]=2[CH:44]=1.C(#N)C.C(OCC)(=O)C>C(O)C(C)C.C1(C)C=CC=CC=1.C(O)C(C)C>[C:2]1([CH3:12])[CH:3]=[CH:4][C:5]([S:8]([OH:11])(=[O:9])=[O:10])=[CH:6][CH:7]=1.[Cl:13][C:14]1[CH:15]=[CH:16][C:17]2[N:26]([C:27]([C:29]3[CH:41]=[CH:40][C:32]([CH2:33][NH:34][C:35]([CH:37]4[CH2:38][CH2:39]4)=[O:36])=[C:31]([F:42])[CH:30]=3)=[O:28])[CH2:25][C:24]3[CH:23]=[N:22][N:21]([CH3:43])[C:20]=3[NH:19][C:18]=2[CH:44]=1