HRID1966977

反应详情

EQUATION

反应方程式

HRID 1966977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

To a solution of 1-cyclopropyl-4-hydroxy-1,4-dihydro-quinoxaline-2,3-dione (31.0 g, 0.14 mol, 1.0 equiv) in N,N-dimethylformamide (250 mL) was added triphenylphosphine (55.9 g, 0.21 mol, 1.5 equiv; [CAS RN 603-35-0]) and the reaction mixture stirred at 135° C. for 4 hours. The reaction mixture was cooled down to 0° C. and dichloromethane (400 mL) was added. The suspension was stirred for 30 min., filtered and washed with dichloromethane (200 mL) providing 23.8 g (83%) of the title compound as a white solid. MS (ISN): m/z=203.1 [M+H]+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled down to 0° C.
  2. stirringThe suspension was stirred for 30 min.
  3. filtrationfiltered
  4. washwashed with dichloromethane (200 mL)