反应 #2434

反应方程式

Ethyl carbamate

glyoxylic acid hydrate

benzotriazole

→

title compound

收率 96.0%

Ethoxycarbonyl-(1-benzotriazolyl)glycine

收率 96.0%

溶剂

toluene

反应条件

后处理

1. 1
   温度the mixture was heated with distillation for 3 h
2. 2
   其他to precipitate the product
3. 3
   workup.ADDITIONThe mixture was diluted with toluene (totally 2.3 1) and
4. 4
   过滤The resultant precipitate was collected by filtration
5. 5
   洗涤washed with toluene (160 ml)
6. 6
   其他dried

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.

来源