HRID1382891
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To a solution of 40 g of 3-(3,5-di-tertiary butyl-4-hydroxyphenyl)-1H-pyrazolo[3,4-b]pyridine in 300 ml of dimethylformamide are added 34,2 g of potassium carbonate and 31 g of 2-acetoxyethyl bromide, and the mixture is stirred at 60° C. for 11 hours. The resulting mixture is poured into ice-cold water and the precipitate is extracted with ethyl acetate and then the extract is washed with water, dried and concentrated. The resulting residue is recrystallized from isopropyl alcohol to give 43 g of 1-(2-acetoxyethyl)-3-(3,5-di-tertiary butyl-4-hydroxyphenyl)-1H-pyrazolo[3,4-b]pyridine as white crystals, melting at 115°-116° C.
WORKUP
后处理
- additionThe resulting mixture is poured into ice-cold water
- extractionthe precipitate is extracted with ethyl acetate
- washthe extract is washed with water
- customdried
- concentrationconcentrated
- customThe resulting residue is recrystallized from isopropyl alcohol