HRID219691

反应详情

EQUATION

反应方程式

HRID 219691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

24.8 g of piperazine (287.9 mmol) were dissolved in 350 ml of ethanol and heated to reflux. 24.9 g of 2-tert-butyl-4-chloro-6-cyclobutyl-pyrimidine (48.06 mmol), dissolved in 50 ml of ethanol, were added dropwise to the solution. The solution was refluxed for further 3 h, cooled to room temperature and then extracted with water and ethyl acetate. The organic layer was washed with 5% citric acid (aq.), and the aqueous layer was adjusted to alkaline pH with 2 N NaOH. The alkaline aqueous layer was reextracted with ethyl acetate, and the organic phase was dried over magnesium sulfate, filtered and concentrated to dryness to yield 8.6 g (65.2%) of the title compound.

WORKUP

后处理

  1. temperatureheated to reflux
  2. additionwere added dropwise to the solution
  3. temperatureThe solution was refluxed for further 3 h
  4. extractionextracted with water and ethyl acetate
  5. washThe organic layer was washed with 5% citric acid (aq.)
  6. dry with materialthe organic phase was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated to dryness