HRID1097592

反应详情

EQUATION

反应方程式

HRID 1097592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-1-[(1S)-1-phenylethyl]-1H-imidazo[4,5-c]quinolin-2-amine hydrobromide (4.0 g, 12 mmol) was treated with ammonia (65 mL of a 7 N solution in methanol) according to the method in Part D of Example 44. The crude product was purified twice by automated flash chromatography (silica cartridge, eluting with aqueous ammonium hydroxide:methanol:dichloromethane in a gradient from 0:0:100 to 0.2:3.8:96). The chromatographed product was washed with diethyl ether several times and dried in a vacuum oven to provide 285 mg of 1-[(1S)-1-phenylethyl]-1H-imidazo[4,5-c]quinoline-2,4-diamine as a brown solid, mp 135-140° C.

WORKUP

后处理

  1. customThe crude product was purified twice by automated flash chromatography (silica cartridge
  2. washeluting with aqueous ammonium hydroxide
  3. washThe chromatographed product was washed with diethyl ether several times
  4. customdried in a vacuum oven