反应详情

Potassium 1,1,2,2-tetrafluoro-4-(methacryloyloxy)butane-1-sulfonate, synthesized as described above, (1.91 g, 5.75 mmol) and phenyl dibenzothiophenium bromide (2.14 g, 6.27 mmol) were added to a 100 mL round bottom flask, along with 15 mL of dichloromethane and 15 mL of distilled, de-ionized water. The mixture was stirred vigorously over the weekend. Stirring was stopped and the mixture separated into two clear layers; the organic layer was washed twice with 30 mL 1% aqueous ammonium hydroxide and five times with 30 mL of distilled, de-ionized water. Hydroquinone (1 mg) was added and dichloromethane was removed by rotary evaporation to yield the product as a white solid (2.41 g, 4.35 mmol). 1H NMR (500 MHz, acetone-d6) δ 8.0 (m, 15H), 6.1 (s, 1H), 5.6 (s, 1H), 4.4 (t, 2H), 3.8 (m, 2H), 1.9 (s, 3H). 19F NMR (300 MHz, acetone-d6) δ −112.7 (s, 2F), −119.8 (s, 2F).

1. distillationof distilled
2. stirringStirring
3. customthe mixture separated into two clear layers
4. washthe organic layer was washed twice with 30 mL 1% aqueous ammonium hydroxide and five times with 30 mL
5. distillationof distilled
6. additionHydroquinone (1 mg) was added
7. customdichloromethane was removed by rotary evaporation