HRID1282158
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
A solution of N-(4-((piperazin-1-yl)methyl)phenylmethyl)acetamide (1.7 g) obtained in Example 88(2), 2-chloro-4,6-dimethylpyrimidine (1.0 g) and potassium carbonate (3.0 g) in acetonitrile (50 ml) was refluxed under heating for 7 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a yellow oil. The obtained yellow oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=20:1) and crystallized from diisopropyl ether and recrystallized from ethyl acetate-hexane to give the title compound (1.1 g) as white crystals.
WORKUP
后处理
- temperatureunder heating for 7 hr
- extractionextracted with ethyl acetate
- washThe extract was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated
- customto give a yellow oil
- customThe obtained yellow oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=20:1)
- customcrystallized from diisopropyl ether
- customrecrystallized from ethyl acetate-hexane