HRID14492
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
- 110 °C
PROCEDURE
实验过程
7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (80 mg, 0.243 mmol) is dissolved in trifluoroacetic acid (1.4 ml), dilute hydrochloric acid (2M, 0.1 ml) is added, and the mixture is heated at 110° C. for 2.5 h. The reaction mixture is cooled to room temperature, diluted with ethyl acetate (50 ml) and washed with saturated sodium bicarbonate solution (2×40 ml), water (40 ml) and saturated brine (40 ml). The organic layer is dried (MgSO4), filtered and evaporated to give a solid. This is triturated with dichloromethane containing a few drops of ethyl acetate and filtered to give a colourless powder.
WORKUP
后处理
- temperatureThe reaction mixture is cooled to room temperature
- washwashed with saturated sodium bicarbonate solution (2×40 ml), water (40 ml) and saturated brine (40 ml)
- dry with materialThe organic layer is dried (MgSO4)
- filtrationfiltered
- customevaporated
- customto give a solid
- customThis is triturated with dichloromethane containing a few drops of ethyl acetate
- filtrationfiltered
- customto give a colourless powder