تفاعل #1563930

معادلة التفاعل

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

(S)-2-methylpropane-2-sulfinamide

→

title compound

المردود 86.4%

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

المردود 86.4%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThe mixture was stirred continuously at 70° C. for 16 h
2. 2
   أخرىReaction mixture
3. 3
   أخرىquenched with saturated aqueous NH4Cl solution
4. 4
   workup.ADDITIONdiluted with ethylacetate
5. 5
   ترشيحfiltered
6. 6
   غسيلThe filtrate was washed with water
7. 7
   أخرىThe organic layer was separated
8. 8
   تجفيفdried over anhydrous sodium sulfate
9. 9
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

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.

المصدر