反应 #1483138

反应方程式

Potassium 1,1,2,2-tetrafluoro-4-(methacryloyloxy)butane-1-sulfonate

triphenylsulfonium bromide

dichloromethane

→

Triphenylsulfonium 1,1,2,2-tetrafluoro-4-(methacryloyloxy)butane-1-sulfonate

收率 80.0%

溶剂

acetonitrile

反应条件

后处理

1. 1
   workup.DISTILLATIONof distilled
2. 2
   workup.STIRRINGStirring
3. 3
   其他the mixture separated into two clear layers
4. 4
   洗涤the organic layer was washed twice with 30 mL 1% aqueous ammonium hydroxide and five times with 30 mL
5. 5
   workup.DISTILLATIONof distilled
6. 6
   workup.ADDITIONHydroquinone (1 mg) was added
7. 7
   其他dichloromethane was removed by rotary evaporation
8. 8
   其他to yield the product as a colorless, viscous oil (2.65 g, 4.76 mmol; 80% yield)

实验过程

Potassium 1,1,2,2-tetrafluoro-4-(methacryloyloxy)butane-1-sulfonate (2.00 g, 6.02 mmol) and triphenylsulfonium bromide (2.25 g, 6.57 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 for 36 hours. 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 colorless, viscous oil (2.65 g, 4.76 mmol; 80% yield). The oil was dissolved in acetonitrile (50 wt %) (3.9 g). 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).

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