HRID1934915

反应详情

EQUATION

反应方程式

HRID 1934915 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 4.03 g of 4-[(3-bromophenyl)amino]-6,7-dimethoxy-3-quinolinecarboxylic acid, 3.24 g of carbonyldiimiazole, and 100 ml of dimethylformamide was heated at 55 for 30 m, cooled to 0° C., and saturated with ammonia gas. After warming to 25 the resulting solution was stirred for 45 m, heated at 50, and evaporated to remove dimethylformamide. The residue was stirred with water, and the resulting solid was filtered, washed with water, and dried. Recrystallization from acetone gave a grey solid, mp 239-242° C.

WORKUP

后处理

  1. temperaturewas heated at 55 for 30 m
  2. temperatureAfter warming to 25 the resulting solution
  3. temperatureheated at 50
  4. customevaporated
  5. customto remove dimethylformamide
  6. stirringThe residue was stirred with water
  7. filtrationthe resulting solid was filtered
  8. washwashed with water
  9. customdried
  10. customRecrystallization from acetone
  11. customgave a grey solid, mp 239-242° C.