HRID1044649

反应详情

EQUATION

反应方程式

HRID 1044649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe synthesis method
  2. extractionextraction
  3. washAfter washing the ether layer with saturated saline
  4. customdrying
  5. distillationthe solvent was distilled away under reduced pressure
  6. customPurification