HRID1601626

反应详情

EQUATION

反应方程式

HRID 1601626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of the above glucuronate in MeOH (24 ml) was added 5% aqueous NaOH (6 ml) and the mixture was left to stir for 20 hours. T.l.c (n-BuOH/acetone/AcOH/5% aq.NH3 /water 45:15:10:10:20) showed that there were two components one of which was M6G and the other morphine. The solution was transferred to a beaker and was acidified with glacial acetic acid (7 ml) which took the pH of the mixture to 5.5. Shortly after this pH was reached (5 minutes), a white solid started to precipitate. The suspension was stirred for a further 30 minutes, the solid filtered and washed with MeOH, and morphine-6-glucuronide (0.4 g, 52%) was obtained after drying at 120° C. for 4 hours, m.p. 240-243° C. More M6G could be obtained by cooling the filtrate.

WORKUP

后处理

  1. waitthe mixture was left
  2. custom(5 minutes)
  3. customto precipitate
  4. stirringThe suspension was stirred for a further 30 minutes
  5. filtrationthe solid filtered
  6. washwashed with MeOH