HRID536499
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
- 150 °C
PROCEDURE
实验过程
1.485 g (4.03 mmol) of 1-(2-fluorobenzyl)-3-iodo-6-methyl-1H-pyrazolo[3,4-d]pyrimidine and 397 mg (4.44 mmol) of copper(I) cyanide were put in 11 ml of absolute DMSO and heated for 2 h at 150° C. After cooling, the reaction mixture was filtered on Celite and then washed with ethyl acetate and THF. The organic phase was washed with 25% aqueous ammonia solution, saturated aqueous ammonium chloride solution and saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated in a rotary evaporator. 994 mg (purity 81%, 75% of theor.) of the target compound was obtained.
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered on Celite
- washwashed with ethyl acetate and THF
- washThe organic phase was washed with 25% aqueous ammonia solution, saturated aqueous ammonium chloride solution and saturated aqueous sodium chloride solution
- dry with materialdried over sodium sulphate
- concentrationconcentrated in a rotary evaporator
- custom994 mg (purity 81%, 75% of theor.) of the target compound was obtained