HRID219691
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated to reflux
- additionwere added dropwise to the solution
- temperatureThe solution was refluxed for further 3 h
- extractionextracted with water and ethyl acetate
- washThe organic layer was washed with 5% citric acid (aq.)
- dry with materialthe organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness