تفاعل #834824

معادلة التفاعل

Chloroethyl vinyl ether

4-Hydroxyphenyldiphenylsulfonium perfluorobutanesulfonate salt

potassium carbonate

N,N,N′,N′-tetramethylethylenediamine

→

4-vinyloxyethoxyphenyldiphenylsulfonium perfluorobutanesulfonate salt

المذيبات

dimethyl sulfoxide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled to 30° C.
2. 2
   أخرىAfter removal of solid
3. 3
   ترشيحthrough filtration, water (100 g)
4. 4
   workup.ADDITIONwas added to the filtrate
5. 5
   غسيلthe aqueous layer was washed three times with hexane (100 g)
6. 6
   workup.ADDITIONTo the washed aqueous layer, dichloromethane (209 g) and water (260 g) were added
7. 7
   workup.STIRRINGunder stirring
8. 8
   استخلاصwhereby the target substance was extracted to the dichloromethane layer
9. 9
   غسيلThe organic layer was repeatedly washed with distilled water until the pH of the separated aqueous layer
10. 10
    أخرىThe solvent was removed by means of a rotary evaporator

الإجراء التجريبي

4-Hydroxyphenyldiphenylsulfonium perfluorobutanesulfonate salt (52.2 g), potassium carbonate (18.0 g), and N,N,N′,N′-tetramethylethylenediamine (1.05 g) were dissolved in dimethyl sulfoxide (26.1 g). Chloroethyl vinyl ether (13.9 g) was added to the solution, followed by heating to 80° C. The reaction mixture was stirred for 15 hours and cooled to 30° C. or lower. After removal of solid through filtration, water (100 g) was added to the filtrate, and the aqueous layer was washed three times with hexane (100 g). To the washed aqueous layer, dichloromethane (209 g) and water (260 g) were added under stirring, whereby the target substance was extracted to the dichloromethane layer. The organic layer was repeatedly washed with distilled water until the pH of the separated aqueous layer was shifted to 7. The solvent was removed by means of a rotary evaporator, to thereby yield 69.9 g of an oily substance. Through 1H-NMR and ion chromatography, the substance was identified to be 4-vinyloxyethoxyphenyldiphenylsulfonium perfluorobutanesulfonate salt.

المصدر