HRID2338

反应详情

EQUATION

反应方程式

HRID 2338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
15 °C

PROCEDURE

实验过程

Ethyl carbamate (69.0 g, 774.5 mmol), glyoxylic acid hydrate (71.3 g, 774.5 mmol) and benzotriazole (92.0 g, 774.5 mmol) were dissolved in toluene (2.3 1) and the mixture was heated with distillation for 3 h to precipitate the product. The mixture was diluted with toluene (totally 2.3 1) and stirred at 15° C. overnight. The resultant precipitate was collected by filtration, washed with toluene (160 ml) and dried to afford the title compound (196.06 g, 96%): mp. 189°-192° C.

WORKUP

后处理

  1. temperaturethe mixture was heated with distillation for 3 h
  2. customto precipitate the product
  3. additionThe mixture was diluted with toluene (totally 2.3 1) and
  4. filtrationThe resultant precipitate was collected by filtration
  5. washwashed with toluene (160 ml)
  6. customdried