Dimethylformamide → HCID 19860705、化合物
反応式
CS([CH2:5][C:6]([F:10])([F:9])[CH:7]=[CH2:8])(=O)=O.[C:11]1([C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:14][O:13]1)=[O:12].[K].C[N:23](C)C=O>>[C:14]1(=[O:13])[N:23]([CH2:5][C:6]([F:10])([F:9])[CH:7]=[CH2:8])[C:11](=[O:12])[C:20]2=[CH:19][CH:18]=[CH:17][CH:16]=[C:15]12参加物
4
反応条件
- 温度
- 110 °C
実験手順
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 stirred 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%).