Acetyl chloride → N-acetyl methacrylamide

Temperature

0 °C

23.7 g of acrylamide and 60 ml of triethylamine were dissolved in 100 ml of dichloromethane in a flask. To the solution was then added dropwise 27.6 g of acetyl chloride at a temperature of −30° C. After the termination of the dropwise addition, the mixture was then stirred at a temperature of 0° C. for 10 hours. Triethylamine hydrochloride thus precipitated was then filtered off. The filtrate was then subjected to distillation under reduced pressure to remove the solvent therefrom. The residue thus obtained was then subjected to column chromatography with ethyl acetate as a developing solvent and silica gel as a filler to obtain 1.5 g of the desired compound (yield: 4%).

1. additionAfter the termination of the dropwise addition
2. customTriethylamine hydrochloride thus precipitated
3. filtrationwas then filtered off
4. distillationThe filtrate was then subjected to distillation under reduced pressure
5. customto remove the solvent
6. customThe residue thus obtained

ORD record

ord-1ae4c6ad69704a90874bb03b4ccd8ab6

Source dataset

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07732550B2