HRID463652

反应详情

EQUATION

反应方程式

HRID 463652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.0 g (29.8 millimoles) of 2-(p-aminophenyl)- 3,4-diazabicyclo[4.1.0]hept-2-en-5-one and 3.9 g (35.9 millimoles) of methoxyacetyl chloride in 150 ml of absolute tetrahydrofuran were refluxed for 4 hours, while stirring. The product was filtered off under suction at 10° C., washed first with tetrahydrofuran and then with water and recrystallized from propanol. 3.5 g (43%) of 2-[p-(methoxyacetylamino)-phenyl]-3,4-diazabicyclo[4.1.0]hept-2-en-5-one were obtained as colorless crystals. Mp.: 206° C.

WORKUP

后处理

  1. filtrationThe product was filtered off under suction at 10° C.
  2. washwashed first with tetrahydrofuran
  3. customwith water and recrystallized from propanol