Hydrochloric Acid → 2-(Vinylsulfonylamino)acetophenone

2-Aminoacetophenone hydrochloride (1.00 g, 5.85 mmol) was dissolved in dichloromethane (50 mL). To the solution was added triethylamine (2.50 mL, 17.9 mmol), and the mixture was stirred at room temperature for 10 minutes. After the reaction mixture wascooled to 0° C., chloroethanesulfonyl chloride (0.92 mL, 8.80 mmol) was added, and the mixture was stirred at the same temperature for 15 minutes. To the reaction mixture was added 2 mol/L hydrochloric acid and the mixture was extracted with chloroform. The organic layer was washed with saturated aqueous sodium chloride and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. To the residue was added a mixed solvent of ethyl acetate and n-hexane for crystallization to obtain 2-(vinylsulfonylamino)acetophenone (0.42 g, 32%).

1. customwascooled to 0° C.
2. stirringthe mixture was stirred at the same temperature for 15 minutes
3. extractionthe mixture was extracted with chloroform
4. washThe organic layer was washed with saturated aqueous sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. customthe solvent was evaporated under reduced pressure
7. additionTo the residue was added a mixed solvent of ethyl acetate and n-hexane
8. customfor crystallization

ORD record

ord-5cd93c65e3044aa8b4c71eb70c7a04c0

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08318782B2