HRID1902608

反应详情

EQUATION

反应方程式

HRID 1902608 的结构方程式

PROCEDURE

实验过程

A mixture of 49.1 g of 1-ethyl-6-methyl-4-hydroxy-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid ethyl ester (0.197 mole) and 250 ml of phosphorus oxychloride is refluxed for 4 hours. Then the excess phosphorus oxychloride is removed by vacuum distillation and the residue is treated with water. The 4-chloro compound (42 g) is filtered under suction and recrystallized from n-hexane, mp 54°-56° C.

WORKUP

后处理

  1. temperatureis refluxed for 4 hours
  2. customThen the excess phosphorus oxychloride is removed by vacuum distillation
  3. additionthe residue is treated with water
  4. filtrationThe 4-chloro compound (42 g) is filtered under suction
  5. customrecrystallized from n-hexane, mp 54°-56° C.