反应详情

温度

95 °C

3 g (14.9 mmol) of 3,4,4-trifluoro-3-butenyl dithiocarbamate in 15 ml of glacial acetic acid are admixed with 2.3 g (15.1 mmol) of chloroacetaldehyde diethyl acetal and 40 mg of p-toluenesulphonic acid monohydrate. The mixture is stirred at 95° C. for 1.5 h and, after cooling to room temperature, is then concentrated by evaporation under reduced pressure. The evaporation residue is taken up in dichloromethane and washed with 1 N sodium hydroxide solution, and the organic phase is removed, dried over Na2SO4 and concentrated by evaporation under reduced pressure. 2.8 g (81.5% of theory; purity by GC/MS: 97.7 area %) of an oil are obtained.

1. temperatureafter cooling to room temperature
2. concentrationis then concentrated by evaporation under reduced pressure
3. washwashed with 1 N sodium hydroxide solution
4. customthe organic phase is removed
5. dry with materialdried over Na2SO4
6. concentrationconcentrated by evaporation under reduced pressure
7. custom2.8 g (81.5% of theory; purity by GC/MS: 97.7 area %) of an oil are obtained