HRID1084834
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- distillationThe solvent was distilled off under reduced pressure
- additionBy adding maleic acid
- customThe obtained crude crystals
- customwere recrystallized from a mixed solvent of ethyl acetate and ethanol