HRID330451

反应详情

EQUATION

反应方程式

HRID 330451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
145 °C

PROCEDURE

实验过程

A solution of 5.0 g of methyl N-(2-chlorophenylsulfonyl)dithiocarbamate in 20 ml of xylene is stirred for 3.5 hours with heating at 145° C. During the heating, methylmercaptan gas is generated. After the reaction is completed, xylene is removed under reduced pressure to yield a pale yellow oil (IR: strong absorption band of -SO2NCS at 1900 cm-1). The oily substance is dissolved in 50 ml of acetonitrile, to which 2.8 g of 2-amino-4-methoxy-6-methylpyrimidine is added and stirred for 30 minutes at 50° C. The precipitated crystals are collected by filtration, and recrystallized from acetonitrile to give 5.6 g of the title compound as a white prism. mp 186.5°~187.5° C.

WORKUP

后处理

  1. customxylene is removed under reduced pressure
  2. customto yield a pale yellow oil (IR: strong absorption band of -SO2NCS at 1900 cm-1)
  3. additionis added
  4. filtrationThe precipitated crystals are collected by filtration
  5. customrecrystallized from acetonitrile