HRID126764

反应详情

EQUATION

反应方程式

HRID 126764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Methylphenylisocyanate (19.0 g.) was added during 10 minutes to a solution of methyl N-[1-amino-1-(methylthio)methylene]carbamate (21.2 g.) in methylene chloride (200 ml.). After 2 hours of stirring, sodium methoxide [obtained by dissolving sodium (3.5 g.) in methanol (30 ml.)] was added at 15°-20° C. The subsequent mixture was stirred at that temperature for 18 hours and the resultant solid collected by filtration and dissolved in water (200 ml.). The solution obtained was acidified with concentrated hydrochloric acid and the solid which formed was collected by filtration, washed well with water and dried to give 3-(4-methylphenyl)-6-methylthiotetrahydro-1,3,5-triazine-2,4-dione (29 g., 81%), m.p. 276°-278° C.

WORKUP

后处理

  1. stirringThe subsequent mixture was stirred at that temperature for 18 hours
  2. filtrationthe resultant solid collected by filtration
  3. dissolutiondissolved in water (200 ml.)
  4. customThe solution obtained
  5. customthe solid which formed
  6. filtrationwas collected by filtration
  7. washwashed well with water
  8. customdried