HRID1833344
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- distillationThe excess phosphorus oxychloride is distilled off in vacuo
- additionthe oily residue is poured on ice
- filtration5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off