HRID261787

反应详情

EQUATION

反应方程式

HRID 261787 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 45 g (0.5 mol) of N-methylthiourea, 54 g (1 mol) of sodium methylate, 200 ml of methanol and 80 g (0.5 mol) of malonic acid diethyl ester was boiled for 3 hours under reflux. 71 g (0.5 mol) of methyl iodide were then added dropwise at about 50° C. and the mixture was stirred for a further 0.5 hour at 50° C. The salt which crystallized out was filtered off and was then dissolved in 400 ml of water. The solution was neutralized by adding glacial acetic acid, the precipitate was then filtered off, and 80 g (93% of theory) of 1,6-dihydro-4-hydroxy-1-methyl-2-methylthio-6-oxo-pyrimidine were thus obtained in the form of a colorless powder of melting point 198° C.

WORKUP

后处理

  1. temperatureunder reflux
  2. customThe salt which crystallized out
  3. filtrationwas filtered off
  4. dissolutionwas then dissolved in 400 ml of water
  5. additionby adding glacial acetic acid
  6. filtrationthe precipitate was then filtered off