HRID129821

反应详情

EQUATION

反应方程式

HRID 129821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1,6-dihydro-5-(4H)-pyrimidinone O-methyloxim monohydrochloride (2.8 g, 17.1 mmol) in dry methanol was added dropwise to a stirred solution of HCl/methanol (49 ml of a 3N solution) and trimethylamine borohydride (1.36 g, 18.7 mmol) at room temperature under a nitrogen atmosphere. After 1 hour the reaction product crystallised spontaneously. Recrystallization from methanol/ethyl acetate gave a light-brown material in 38% yield (1.30 g). Mp. 214.0° C.

WORKUP

后处理

  1. customAfter 1 hour the reaction product crystallised spontaneously
  2. customRecrystallization from methanol/ethyl acetate
  3. customgave a light-brown material in 38% yield (1.30 g)