HRID1382894

反应详情

EQUATION

反应方程式

HRID 1382894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.7 g of the compound of Example 43 in 20 ml of chloroform is added 1.5 g of triethylamine, and to the mixture with stirring at -10°--2° C. is added 1.4 g of ethyl chlorocarbonate dropwise. After completion of the addition, the whole mixture is stirred at 0° C. for 3 hours, and then at room temperature for 2 hours. The reaction solution is washed with water, dried and concentrated, and then the resulting residue is recrystallized from isopropyl ether to give 3.8 g of 3-(3,5-di-tertiary butyl-4-hydroxyphenyl)-1-(2-ethoxycarbonyloxyethyl)-1H-pyrazolo[3,4-b]-pyridine as white crystals, melting at 103°-105° C.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. stirringthe whole mixture is stirred at 0° C. for 3 hours
  3. washThe reaction solution is washed with water
  4. customdried
  5. concentrationconcentrated
  6. customthe resulting residue is recrystallized from isopropyl ether