反应详情

温度

135 °C

To a solution of methyl N-[(5-acetyl-2-chlorophenyl)methyl]carbamate (10 g, 41.5 mmol) (prepared by the method given in European Patent Publication EP 1586552) in toluene was added N,N-dimethylformamide dimethyl acetal (9.88 g, 82.9 mmol) and the reaction mixture was heated at 135° C. for 2 days. TLC analysis (50% ethyl acetate/pet ether) showed the reaction was complete. The solvent was evaporated under vacuum and water was added to the residue. The water layer was extracted with ethyl acetate three times. The combined the organic phases were washed with water, brine, dried over Na2SO4 and concentrated under vacuum to give the title compound (10 g, 81% yield) as solid.

1. customThe solvent was evaporated under vacuum and water
2. additionwas added to the residue
3. extractionThe water layer was extracted with ethyl acetate three times
4. washwere washed with water, brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under vacuum