HRID387877

反应详情

EQUATION

反应方程式

HRID 387877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

After mixing 6-carbamoyl-4-chloro-7-methoxyquinoline (2.0 g, 8.4509 mmol), 5-hydroxyindole (1.68 g), diisopropylethylamine (2.2 ml) and N-methylpyrrolidone (2.2 ml), the mixture was heated and stirred at 150° C. for 5 hours. After cooling, the solidified part of the reaction solution was dissolved in dimethylsulfoxide and then adsorbed onto NH silica gel and purified by NH silica gel column chromatography (ethyl acetate-methanol system). The obtained crystals were suspended in ethanol, the suspension was diluted with diethyl ether and hexane, and the crystals were filtered out, washed with diethyl ether:hexane=1:5 and dried by aspiration to obtain the title compound (1.291 g, 3.8698 mmol, 45.79%) as light yellow crystals.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureAfter cooling
  3. custompurified by NH silica gel column chromatography (ethyl acetate-methanol system)
  4. additionthe suspension was diluted with diethyl ether and hexane
  5. filtrationthe crystals were filtered out
  6. washwashed with diethyl ether
  7. dry with materialhexane=1:5 and dried by aspiration