HRID2170802

反应详情

EQUATION

反应方程式

HRID 2170802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(4-Chloro-phenyl)-5-methyl-3H-pyrimidin-4-one (570 mg, 2.58 mmol) was suspended in phosphorus oxychloride (2 ml) and heated to reflux for 2 hours. The mixture was cooled before being stripped to dryness in vacuo. The resulting crude product was solubilised in water (10 ml) and ethyl acetate (10 ml) and the biphasic mixture separated. The aqueous layer was further extracted with ethyl acetate (10 ml) before the combined organics were dried with magnesium sulphate, filtered and stripped to dryness in vacuo to give 6-Chloro-2-(4-chloro-phenyl)-5-methyl-1,6-dihydro-pyrimidine as a white solid (567 mg, 2.38 mmol, 92% yield).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 2 hours
  3. temperatureThe mixture was cooled
  4. customethyl acetate (10 ml) and the biphasic mixture separated
  5. extractionThe aqueous layer was further extracted with ethyl acetate (10 ml) before the combined
  6. dry with materialorganics were dried with magnesium sulphate
  7. filtrationfiltered