反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of 9H-carbazole-1-carboxylic acid (148 mg) and 1-hydroxybenzotriazole (130 mg) in dichloromethane (3 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (201 mg) and the mixture was stirred for 5 minutes. After adding 4-methyl-3-(pyrimidin-5-yl)aniline (130 mg) and 4-dimethylaminopyridine (128 mg), the mixture was stirred for 24 hours. The mixture was diluted with dichloromethane and washed with water and brine. The organic layer was dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by a silica gel column chromatography eluting with 2% methanol in dichloromethane to give N-(4-methyl-3-(pyrimidin-5-yl)-phenyl)-9H-carbazole-1-carboxamide (140 mg, 52.8%).
WORKUP
后处理
- stirringthe mixture was stirred for 24 hours
- washwashed with water and brine
- dry with materialThe organic layer was dried over magnesium sulfate
- customevaporated under reduced pressure
- customThe residue was purified by a silica gel column chromatography
- washeluting with 2% methanol in dichloromethane