Dimethylamine → Cyclohexanecarboxamide, N,N-dimethyl-2-oxo-

Temperature

0 °C

0.313 mol (50 ml) of ethyl cyclohexanone-2-carboxylate and 140 ml 33% dimethylamine in ethanol (about 0.78 mol dimethylamine) were stirred in a pressure reactor for 12 hours at 110° C. After cooling the reaction mixture was concentrated on a rotary evaporator, the residue was dissolved in 500 ml ethyl acetate and the organic phase was washed with 200 ml of 1 M NaOH and 3×50 ml water. The organic phase was then evaporated on a rotary evaporator to dryness. 46 g of the crude product was dissolved in 100 ml tert-butyl methyl ether and cooled to 0° C. Precipitated product was filtered off and dried, 3.6 g of the title compound were obtained.

1. temperatureAfter cooling the reaction mixture
2. concentrationwas concentrated on a rotary evaporator
3. dissolutionthe residue was dissolved in 500 ml ethyl acetate
4. washthe organic phase was washed with 200 ml of 1 M NaOH and 3×50 ml water
5. customThe organic phase was then evaporated on a rotary evaporator to dryness
6. dissolution46 g of the crude product was dissolved in 100 ml tert-butyl methyl ether
7. filtrationPrecipitated product was filtered off
8. customdried

ORD record

ord-7fcb3ebf32264ef9be1f51155be7ca9b

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09394324B2