HRID1678459
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
[2-Methyl-3′-(4-morpholin-4-yl-phenylcarbamoyl)-biphenyl-4-yl]-carbamic acid tert-butyl ester (670 mg) was stirred in methanol (15 ml) and 5M HCl (5 ml) at 20 C for 2 days. TLC indicated that the reaction was progressing slowly and so the mixture was heated to reflux for 6 h. The reaction was allowed to cool and was then basified and extracted with dichloromethane. The dried extract was evaporated and the residue purified on silica gel. Elution with dichloromethane:ethanol:0.880 ammonia; 400:8:1 gave a colourless foam which crystallized on standing (354 mg).
WORKUP
后处理
- temperatureso the mixture was heated
- temperatureto reflux for 6 h
- temperatureto cool
- extractionextracted with dichloromethane
- extractionThe dried extract
- customwas evaporated
- customthe residue purified on silica gel
- washElution with dichloromethane
- custom400:8:1 gave a colourless foam which
- customcrystallized