HRID1382889

反应详情

EQUATION

反应方程式

HRID 1382889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 45.2 g of 4-(2-chloronicotinoyl)2,6-di-tertiary butylphenol and 21 g of 2-hydrazinoethanol in 230 ml of pyridine is refluxed under stirring for 18 hours. After completion of the reaction, the pyridine is concentrated and 140 ml of ethanol and 70 ml of water are added to the residue. The mixture is warmed to dissolve and then cooled to 0° C. The precipitated crystals are collected by filtration, recrystallized from 70% dioxane and then dried to give 40 g of 3-(3,5-di-tertiary butyl-4-hydroxyphenyl)-1-(2-hydroxyethyl)-1H-pyrazolo[3,4-b]pyridine, melting at 135°-137° C.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. concentrationthe pyridine is concentrated
  3. addition140 ml of ethanol and 70 ml of water are added to the residue
  4. temperatureThe mixture is warmed
  5. dissolutionto dissolve
  6. filtrationThe precipitated crystals are collected by filtration
  7. customrecrystallized from 70% dioxane
  8. customdried