HRID2416556
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 mixture of compound of Example 34 (0.35 g, 0.435 mmol) and 2-formyl-4,4-dimethoxy-butyronitrile (0.30 g, 1.91 mmol) in CH3CN was added trifluoroacetic acid (0.33 mL, 4.35 mmol). The mixture was heated to 60° C. for 18 hours and additional 2-formyl-4,4-dimethoxy-butyronitrile (0.15 g, 0.186 mmol) and trifluoroacetic acid (0.15 mL, 1.95 mmol) were added. The mixture is was heated to 60° C. for 18 hours before being cooled, diluted with ethyl acetate, washed with sat. aq. NaHCO3, water, brine, and dried over MgSO4. Concentration and chromatography (silica gel, 98:2:0.3 dichloromethane/methanol/conc. NH4OH) gave 0.16 g (41%) of the title compound. MS 880 (M+H)+.
WORKUP
后处理
- temperatureThe mixture is was heated to 60° C. for 18 hours
- temperaturebefore being cooled
- washwashed with sat. aq. NaHCO3, water, brine
- dry with materialdried over MgSO4
- concentrationConcentration and chromatography (silica gel, 98:2:0.3 dichloromethane/methanol/conc. NH4OH)