反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The synthesis method shall be explained concretely following the order below. 2,4,6-trichloropyrimidine (20 ml, 165 mmol) and triethylamine (27.7 ml) were dissolved in ether (200 ml), and phenylpiperadine (25.2 ml, 165 mmol) was added under ice cooling. After approximately 1 hour of agitation at room temperature, water was added, and extraction was carried out 2 times with ether. After washing the ether layer with saturated saline, drying was done with MgSO4, and the solvent was distilled away under reduced pressure. Purification was done by silica gel chromatography (hexane:ethyl acetate=19:1), and 17.6 g (34% yield) of 4,6-dichloro-2-(4-phenylpiperazin-1-yl)pyrimidine was obtained. NMR data for the obtained 4,6-dichloro-2-(4-phenylpiperazin-1-yl)pyrimidine is shown below.
WORKUP
后处理
- customThe synthesis method
- extractionextraction
- washAfter washing the ether layer with saturated saline
- customdrying
- distillationthe solvent was distilled away under reduced pressure
- customPurification