HRID1097592
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe crude product was purified twice by automated flash chromatography (silica cartridge
- washeluting with aqueous ammonium hydroxide
- washThe chromatographed product was washed with diethyl ether several times
- customdried in a vacuum oven