HRID606121

反应详情

EQUATION

反应方程式

HRID 606121 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 4-chloro-1-{2-[3-(4-fluorophenyl)isoxazol-5-yl]ethyl}-2-propyl-1H-imidazo[4,5-c]quinoline (1.22 g, 2.81 mmol) and 7 N ammonia in methanol (100 mL) was sealed in a pressure vessel and heated at 150° C. for 12 hours and allowed to cool to room temperature. The volatiles were removed under reduced pressure, and the crude product was purified by column chromatography on silica gel (eluting with 10% to 15% CMA in chloroform). The product was then triturated sequentially with toluene and hexane/diethyl ether to provide 0.312 g of 1-{2-[3-(4-fluorophenyl)isoxazol-5-yl]ethyl}-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine as a white powder, mp 208.0-209.0° C.

WORKUP

后处理

  1. customwas sealed in a pressure vessel
  2. temperatureto cool to room temperature
  3. customThe volatiles were removed under reduced pressure
  4. customthe crude product was purified by column chromatography on silica gel (eluting with 10% to 15% CMA in chloroform)
  5. customThe product was then triturated sequentially with toluene and hexane/diethyl ether