HRID1021009

反应详情

EQUATION

反应方程式

HRID 1021009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium 1,1,2,2-tetrafluoro-4-(methacryloyloxy)butane-1-sulfonate (2 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, deionized water. The mixture was vigorously stirred for 36 hours. Stirring was stopped and the mixture separated into two clear layers; the organic layer was washed twice with 30 mL of 1% (w/w) aqueous ammonium hydroxide and five times with 30 mL of distilled, de-ionized water. The organic layer was dried over sodium sulfate and filtered. Hydroquinone (1 mg) was added and the solvent was removed by rotary evaporation and high vacuum to yield the product as a colorless, viscous oil (2.65 g, 4.76 mmol). 1H NMR (d6-acetone): 7.9 (br), 6.1 (s), 5.6 (s), 4.4 (t), 2.8 (m), 1.9 (s); 19F NMR (d6-acetone): −112.7 (s), −119.7 (s).

WORKUP

后处理

  1. distillationof distilled
  2. stirringStirring
  3. customthe mixture separated into two clear layers
  4. washthe organic layer was washed twice with 30 mL of 1% (w/w) aqueous ammonium hydroxide and five times with 30 mL
  5. distillationof distilled
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. filtrationfiltered
  8. additionHydroquinone (1 mg) was added
  9. customthe solvent was removed by rotary evaporation and high vacuum