HRID1678459

反应详情

EQUATION

反应方程式

HRID 1678459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureso the mixture was heated
  2. temperatureto reflux for 6 h
  3. temperatureto cool
  4. extractionextracted with dichloromethane
  5. extractionThe dried extract
  6. customwas evaporated
  7. customthe residue purified on silica gel
  8. washElution with dichloromethane
  9. custom400:8:1 gave a colourless foam which
  10. customcrystallized