HRID423271

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID1146

Trimethylamine

C3H9N

HCID11066000

未命名化合物

HCID66676455

未命名化合物

PRODUCTS

生成物

结构：CCOC(=O)CCc1ccc(NC(=O)c2ccccc2-c2ccc(C(F)(F)F)cc2)c(C(=O)N(C)C)c1

HCID66676801

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8857

Ethyl acetate

C4H8O2

CONDITIONS

反应条件

温度: 0 °C

PROCEDURE

实验过程

3-(4-Amino-3-dimethylcarbamoylphenyl)propionic acid ethyl ester (1.52 g) was dissolved in ethyl acetate (10 mL), and trimethylamine (533 mg) was added thereto. After cooling down to 0° C., 4′-trifluoromethylbiphenyl-2-carbonyl chloride (synthesized from the corresponding carboxylic acid 0.529 g) was added thereto, and the mixture was stirred at room temperature overnight. After filtration of the insoluble material, the filtrate was concentrated and purified by column chromatography on silica gel (ethyl acetate:hexane=3:2, v/v) to give the title compound (0.843 g).

WORKUP

后处理

additionwas added
filtrationAfter filtration of the insoluble material
concentrationthe filtrate was concentrated
custompurified by column chromatography on silica gel (ethyl acetate

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-f8c63a0f87ab4de8b4e1b78ed2642a8f
来源数据集: uspto-grants-2012_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08101774B2
来源说明: uspto-grants-2012_01

反应 SMILES

[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[C:9]([C:14](=[O:18])[N:15]([CH3:17])[CH3:16])[CH:8]=1)[CH3:2].CN(C)C.[F:24][C:25]([F:42])([F:41])[C:26]1[CH:31]=[CH:30][C:29]([C:32]2[C:33]([C:38](Cl)=[O:39])=[CH:34][CH:35]=[CH:36][CH:37]=2)=[CH:28][CH:27]=1>C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:38]([C:33]2[C:32]([C:29]3[CH:30]=[CH:31][C:26]([C:25]([F:24])([F:41])[F:42])=[CH:27][CH:28]=3)=[CH:37][CH:36]=[CH:35][CH:34]=2)=[O:39])=[C:9]([C:14](=[O:18])[N:15]([CH3:16])[CH3:17])[CH:8]=1)[CH3:2]