HRID660883

反应详情

EQUATION

反应方程式

HRID 660883 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

159 mg (0.39 mmol) of the compound from Example 147A in 4 ml methanol are treated with 1.57 ml of a 1 N solution of lithium hydroxide in water (1.57 mmol) and the resulting mixture is stirred overnight at RT. The methanol is removed on the rotary evaporator, the residue diluted with water and the resulting aqueous phase extracted twice with dichloromethane. These organic phases are discarded. The aqueous phase is then acidified with 1 N hydrochloric acid and extracted three times with dichloromethane. The extracts are combined, dried over magnesium sulphate, freed of solvent on the rotary evaporator and the residue dried under high vacuum. 144 mg (94% of theory) of the title compound are obtained.

WORKUP

后处理

  1. customThe methanol is removed on the rotary evaporator
  2. additionthe residue diluted with water
  3. extractionthe resulting aqueous phase extracted twice with dichloromethane
  4. extractionextracted three times with dichloromethane
  5. dry with materialdried over magnesium sulphate
  6. customfreed of solvent on the rotary evaporator
  7. customthe residue dried under high vacuum