HRID26278

反应详情

EQUATION

反应方程式

HRID 26278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,2,3,4,5,6-hexahydro-6-methyl-8-methoxy-11-oxo-2,6-methano-3-benzazocine (2.18 g.) and hydrobromic acid (48%, 20 ml.) was stirred under reflux (for 30 min.), basified with dilute ammonia and extracted with chloroform. Desiccation and concentration of the chloroform extracts afforded a tan solid (1.1 g.), recrystallization of which from acetone afforded 1,2,3,4,-5,6-hexahydro-6-methyl-8-hydroxy-11-oxo-2,6-methano-3-benzazocine (III: R=CH3, X"=HO, Y+Z=O; 0.4 g.), a white solid.

WORKUP

后处理

  1. temperatureunder reflux (for 30 min.)
  2. extractionextracted with chloroform
  3. customDesiccation and concentration of the chloroform extracts afforded
  4. customa tan solid (1.1 g.), recrystallization of which from acetone