تفاعل #1483134

معادلة التفاعل

Triethylammonium 1,1-difluoro-2-(methacryloyl-oxy)ethane-1-sulfonate

(t-butylphenyl)(diphenyl)sulfonium bromide

dichloromethane

→

oil

المردود 87.5%

(t-butylphenyl)(diphenyl)sulfonium 1,1-difluoro-2-(methacryloyloxy)ethane-1-sulfonate

المردود 87.5%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGStirring
2. 2
   أخرىthe mixture separated into two clear layers
3. 3
   غسيلthe organic layer was washed once with 30 mL 0.1% aqueous hydrochloric acid and four times with 30 mL of de-ionized water
4. 4
   workup.ADDITIONHydroquinone (1 mg) was added
5. 5
   أخرىdichloromethane was removed by rotary evaporation

الإجراء التجريبي

Triethylammonium 1,1-difluoro-2-(methacryloyl-oxy)ethane-1-sulfonate (5.00 g, 15.1 mmol) and (t-butylphenyl)(diphenyl)sulfonium bromide (6.00 g, 15.0 mmol) were added to a 100 mL round bottom flask, along with 30 mL of dichloromethane and 30 mL of de-ionized water. The mixture was stirred vigorously overnight. Stirring was stopped and the mixture separated into two clear layers; the organic layer was washed once with 30 mL 0.1% aqueous hydrochloric acid and four times with 30 mL of de-ionized water. Hydroquinone (1 mg) was added and dichloromethane was removed by rotary evaporation to yield the product as a colorless, viscous oil (7.2 g, 87% yield). The oil was dissolved to 40 wt % in acetonitrile for further use. 1H NMR (500 MHz, acetone-d6) δ 7.9 (m, 14H), 6.1 (s, 1H), 5.7 (s, 1H), 4.7 (m, 2H), 1.9 (s, 3H), 1.3 (s, 9H). 19F NMR (300 MHz, acetone-d6) δ −115.7 (s, 2F).

المصدر