HRID1902608
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureis refluxed for 4 hours
- customThen the excess phosphorus oxychloride is removed by vacuum distillation
- additionthe residue is treated with water
- filtrationThe 4-chloro compound (42 g) is filtered under suction
- customrecrystallized from n-hexane, mp 54°-56° C.