HRID1605840

反应详情

EQUATION

反应方程式

HRID 1605840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 148 parts of methyl N-(1-amino-1-methylthiomethylene)-carbamate, prepared as in Example 2, in 2,000 parts methylene chloride is added 154 parts of p-chlorophenyl isocyanate. The reaction is stirred for 3 days. Then to it is added 54 parts of sodium methoxide in 540 parts of methanol. The reaction mixture is then refluxed for 1 hour. The reaction mass is cooled, and 2,000 parts of ether are added. The solid collected by filtration is dissolved in water and the solution neutralized with hydrochloric acid. The new solid thus formed is collected, dried, and recrystallized from ethanol/H2O to give 140 parts of 3-(p-chlorophenyl)-6-methylthio-s-triazine-2,4(1H,3H)-dione melting at 292°-295°C.

WORKUP

后处理

  1. temperatureThe reaction mixture is then refluxed for 1 hour
  2. temperatureThe reaction mass is cooled
  3. filtrationThe solid collected by filtration
  4. dissolutionis dissolved in water
  5. customThe new solid thus formed
  6. customis collected
  7. customdried
  8. customrecrystallized from ethanol/H2O