تفاعل #2434

معادلة التفاعل

Ethyl carbamate

glyoxylic acid hydrate

benzotriazole

→

title compound

المردود 96.0%

Ethoxycarbonyl-(1-benzotriazolyl)glycine

المردود 96.0%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated with distillation for 3 h
2. 2
   أخرىto precipitate the product
3. 3
   workup.ADDITIONThe mixture was diluted with toluene (totally 2.3 1) and
4. 4
   ترشيحThe resultant precipitate was collected by filtration
5. 5
   غسيلwashed with toluene (160 ml)
6. 6
   أخرىdried

الإجراء التجريبي

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.

المصدر