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 was cooled to 0° C., chloroethanesulfonyl chloride (0.92 mL, 8.80 mmol) was added to the mixture, 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 then 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. temperatureAfter the reaction mixture was cooled 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レコード

ord-584e886578ee47e49264f1a5929a0d1c

出典データセット

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07425636B2