HRID1084834

反应详情

EQUATION

反应方程式

HRID 1084834 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In 70 ml of dimethylformamide were suspended 4.0 g of 1-(3-hydroxyphenyl)-3-phenyl-1H-pyrazolo[3,4-b]pyridine, 2.6 g of 3-dimethylamino-2-methylpropylchloride and 2.3 g of potassium carbonate. The mixture was stirred at 100° C. for 6 hours. The solvent was distilled off under reduced pressure. By adding maleic acid, the residue was converted into the salt. The obtained crude crystals were recrystallized from a mixed solvent of ethyl acetate and ethanol to give 5.2 g of 1-[3-(3-dimethylamino-2-methylpropoxy)phenyl]-3-phenyl-1H-pyrazolo[3,4-b]pyridine·maleate, m.p. 134°-136° C.

WORKUP

后处理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionBy adding maleic acid
  3. customThe obtained crude crystals
  4. customwere recrystallized from a mixed solvent of ethyl acetate and ethanol