Potassium Carbonate → 2-cyclopropyl-N-methoxy-N-methylacetamide

Temperature

0 °C

Oxalyl chloride (9.6 ml) was added dropwise at 0° C. under nitrogen to a stirred solution of cyclopropaneacetic acid (10 g) in dichloromethane (250 ml), then the mixture was stirred at 0° C. for 1 hour and at ambient temperature for 42 hours. The resulting solution of cyclopropaneacetyl chloride was added dropwise at 0-5° C. to a stirred aqueous solution of N,O-dimethylhydroxylamine prepared by addition of potassium carbonate (24.8 g) in portions at 0-5° C. over 30 minutes to a stirred solution of N,O-dimethylhydroxylamine hydrochloride (10.2 g) in water (110 ml). When the addition of the acid chloride solution was complete, the mixture was stirred at 0° C. for 20 minutes and at ambient temperature for 4 hours. The organic phase was separated, washed with saturated aqueous sodium chloride solution (50 ml) and dried (MgSO4), then the solvent was removed in vacuo to leave N-methoxy-N-methylcyclopropaneacetamide (13.6 g) as a colourless oil which was used without further purification.

1. stirringthe mixture was stirred at 0° C. for 20 minutes and at ambient temperature for 4 hours
2. customThe organic phase was separated
3. washwashed with saturated aqueous sodium chloride solution (50 ml)
4. dry with materialdried (MgSO4)
5. customthe solvent was removed in vacuo

ORD record

ord-532cbddbad1e46229e4ea57530e4ec32

Source dataset

uspto-grants-2005_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06900216B2