反应详情

温度

110 °C

The compound 1-methanesulfonyl-2,2-difluoro-3-butene (11.2 g, 60.2 mM), potassium phthalide (12.3 g, 66.4 mM) and dry dimethylformamide (30 mL) are strirred and heated (bath temperature 110° C.) under nitrogen for 120 hours. After cooling to room temperature, the crude reaction product is precipitated by the addition of water (approximately 300 mL), filtered and dissolved in dichloromethane. The dichloromethane solution is washed with 1N potassium hydroxide (twice), water (twice), dried (Na2SO4) and evaporated to yield 1-phthalimido-2,2-difluoro-3-butene as beige-colored crystals: 11.9 g (83%).

1. temperatureAfter cooling to room temperature
2. customthe crude reaction product
3. customis precipitated by the addition of water (approximately 300 mL)
4. filtrationfiltered
5. dissolutiondissolved in dichloromethane
6. washThe dichloromethane solution is washed with 1N potassium hydroxide (twice), water (twice),
7. dry with materialdried (Na2SO4)
8. customevaporated