HRID1833342

反应详情

EQUATION

反应方程式

HRID 1833342 的结构方程式

PROCEDURE

实验过程

200 g. of 2-methylpyrazolo[1,5-a]pyrido[3,4-e]-pyrimidin-5(4H)-one of Example 1c are refluxed with 800 ml. of phosphorus oxychloride overnight. The excess phosphorus oxychloride is removed in vacuo and the oily residue decomposed by pouring on ice. The acidic aqueous solution is made alkaline with sodium hydroxide. The precipitated 5-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off, yield: 143 g. (66%); m.p. 169.8° (ethyl acetate).

WORKUP

后处理

  1. customThe excess phosphorus oxychloride is removed in vacuo
  2. additionby pouring on ice
  3. filtrationThe precipitated 5-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off