HRID219695

反应详情

EQUATION

反应方程式

HRID 219695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

25.1 g of piperazine (291.4 mmol) were dissolved in 100 ml of ethanol and heated to 50° C. 17 g of 2-tert-butyl-4-chloro-6-cyclopropyl-pyrimidine (81 mmol), dissolved in 100 ml of ethanol, were added dropwise within 2 h. After heating to reflux at 70° C. for 5 h the reaction mixture was stirred at room temperature overnight. The ethanol was evaporated and the residue suspended in 200 ml of water. The aqueous phase was extracted 4 times with 100 ml of dichloromethane each. Drying over magnesium sulfate, filtration, and evaporation to dryness gave 19.2 g (90.9%) of the title compound.

WORKUP

后处理

  1. additionwere added dropwise within 2 h
  2. temperatureAfter heating
  3. temperatureto reflux at 70° C. for 5 h the reaction mixture
  4. customThe ethanol was evaporated
  5. extractionThe aqueous phase was extracted 4 times with 100 ml of dichloromethane each
  6. dry with materialDrying over magnesium sulfate, filtration, and evaporation to dryness