HRID1833344

反应详情

EQUATION

反应方程式

HRID 1833344 的结构方程式

PROCEDURE

实验过程

23.5 g. of 8-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one of Example 1b are refluxed in 100 ml. of phosphorus oxychloride for 12 hours. The excess phosphorus oxychloride is distilled off in vacuo and the oily residue is poured on ice. After standing for 1 hour, 5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off, yield: 17 g. (67%); m.p. 203.4° (ethyl acetate).

WORKUP

后处理

  1. distillationThe excess phosphorus oxychloride is distilled off in vacuo
  2. additionthe oily residue is poured on ice
  3. filtration5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off