反应详情

温度

10 °C

A 1000-mL round bottom flask equipped with a mechanical stirrer, thermometer and addition funnel was charged with 2-(dimethylamino)-N-hydroxy-2-oxoethanimidoyl chloride (94.0 g, 0.62 mol) and a solution of 2,6-difluorostyrene (84.0 g, 0.60 mol) in chlorobenzene (275 g). The reaction mixture was cooled to 10° C., and a solution of potassium bicarbonate (70 g, 0.70 mol) in water (350 mL) was added dropwise over 1 h while maintaining the reaction temperature between 10 to 15° C. When gas chromatography analysis of the reaction mixture showed about 3% of 2-(dimethylamino)-N-hydroxy-2-oxo-ethanimidoyl chloride remaining, water (200 mL) was added to the reaction mixture. The layers were separated, and the organic layer was washed with water (300 mL) and concentrated under reduced pressure. Toluene was added to the resulting residu, and the mixture was again concentrated under reduced pressure to provide the title compound as an oil (144 g).

1. customA 1000-mL round bottom flask equipped with a mechanical stirrer
2. additionthermometer and addition funnel
3. temperaturewhile maintaining the reaction temperature between 10 to 15° C
4. additionwas added to the reaction mixture
5. customThe layers were separated
6. washthe organic layer was washed with water (300 mL)
7. concentrationconcentrated under reduced pressure
8. additionToluene was added to the resulting residu
9. concentrationthe mixture was again concentrated under reduced pressure