HRID2287462

反应详情

EQUATION

反应方程式

HRID 2287462 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8-[3-(N-glycyl-N-methylamino)-2,6-dichlorobenzyloxy]-4-(imidazol-1-yl)-2-methylquinoline (80 mg), 4-(dimethylcarbamoyl)cinnamic acid (41 mg) and 1-hydroxybenzotriazole (29.9 mg) in dichloromethane (0.8 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (39.1 mg) at ambient temperature, and the mixture was stirred for 3 hours at the same temperature. To the mixture was added saturated sodium bicarbonate solution, and the separated organic layer was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by preparative thin layer chromatography (chloroform:methanol, 10:1, v/v) to give 8-[2,6-dichloro-3-[N-[4-(dimethylcarbamoyl)cinnamoylglycyl]-N-methylamino]benzyloxy]-4-(imidazol-1-yl)-2-methylquinoline (104 mg) as colorless amorphous.

WORKUP

后处理

  1. dry with materialthe separated organic layer was dried over magnesium sulfate
  2. customevaporated in vacuo
  3. customThe residue was purified by preparative thin layer chromatography (chloroform