HRID1097600
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
tert-Butyl 2-(2-amino-4-chloro-1H-imidazo[4,5-c]quinolin-1-yl)ethylcarbamate (3.5 g, 9.7 mmol) and ammonia (approximately 100 mL of a 7 N solution in methanol) were added to a pressure vessel, which was sealed and heated at 150° C. overnight. The volatiles were removed under reduced pressure, and the residue was purified by automated flash chromatography (silica cartridge, eluting with aqueous ammonium hydroxide:methanol:dichloromethane in a gradient from 0:0:100 to 1.5:28.5:70) to provide 840 mg of 1-(2-aminoethyl)-1H-imidazo[4,5-c]quinoline-2,4-diamine as a dark grey solid.
WORKUP
后处理
- customwhich was sealed
- customThe volatiles were removed under reduced pressure
- customthe residue was purified by automated flash chromatography (silica cartridge
- washeluting with aqueous ammonium hydroxide