HRID224583

反应详情

EQUATION

反应方程式

HRID 224583 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 38 g (0.44 mol) of cyanacetic acid, 200 ml of acetic anhydride and 200 ml of acetic acid was added 60 g of 1-methyl-3-phenylurea. The solution was stirred at 90°-100° C. for some hours. After cooling, 65.5 g of 1-cyanoaceto-1-methyl-3-phenylurea (XV) was filtered off (mp 180° C). This was dissolved in 3 1 of boiling ethanol and 10 ml of 10% soda solution was added. After cooling and filtration, the filtrate was evaporated and the crystals were washed with ethanol. Yield 46.7 g (XVI) NMR.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtration65.5 g of 1-cyanoaceto-1-methyl-3-phenylurea (XV) was filtered off (mp 180° C)
  3. dissolutionThis was dissolved in 3 1 of boiling ethanol and 10 ml of 10% soda solution
  4. additionwas added
  5. temperatureAfter cooling
  6. filtrationfiltration
  7. customthe filtrate was evaporated
  8. washthe crystals were washed with ethanol