반응 #1563930

반응 방정식

4-chloro-1-(2,5-difluorophenyl)butan-1-one

(S)-2-methylpropane-2-sulfinamide

→

title compound

수율 86.4%

(S,E)-N-(4-chloro-1-(2,5-difluorophenyl)butylidene)-2-methylpropane-2-sulfinamide

수율 86.4%

용매

THF

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred continuously at 70° C. for 16 h
2. 2
   기타Reaction mixture
3. 3
   기타quenched with saturated aqueous NH4Cl solution
4. 4
   workup.ADDITIONdiluted with ethylacetate
5. 5
   여과filtered
6. 6
   세척The filtrate was washed with water
7. 7
   기타The organic layer was separated
8. 8
   건조dried over anhydrous sodium sulfate
9. 9
   농축concentrated under reduced pressure

실험 절차

Titanium (IV) ethoxide (54.77 g, 240.13 mmol) was added to a solution of 4-chloro-1-(2,5-difluorophenyl)butan-1-one (35 g, 160.09 mmol) and (S)-2-methylpropane-2-sulfinamide (29.1 g, 240.13 mmol) in THF (400 mL) with stirring. The mixture was stirred continuously at 70° C. for 16 h. Reaction mixture was then cooled to a temperature of 20-35° C., quenched with saturated aqueous NH4Cl solution, diluted with ethylacetate and filtered. The filtrate was washed with water followed by brine solution. The organic layer was separated, dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford 44.5 g of the title compound as a colourless liquid.

출처