反应详情

To 700 mg of 5-carbamoylmethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide were added 21 ml of ethanol, 7 ml of 1 mol/l aqueous solution of sodium hydroxide, and the mixture was refluxed for 18 hours. The reaction mixture was poured into water, washed with ethyl acetate, and further the aqueous layer was adjusted to pH value of 1 to 2 with 2 mol/l hydrochloric acid, which was then extracted with ethyl acetate. The organic layer was washed with water and saturated brine in sequence and dried again over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue obtained was suspended with diethyl ether to collect the crystals by filtration. The crystals obtained were recrystallized from methylene chloride to obtain 435 mg of aimed product as colorless crystals.

1. temperaturethe mixture was refluxed for 18 hours
2. washwashed with ethyl acetate
3. extractionwas then extracted with ethyl acetate
4. washThe organic layer was washed with water and saturated brine in sequence
5. dry with materialdried again over anhydrous sodium sulfate
6. distillationSolvent was distilled off under reduced pressure
7. customthe residue obtained
8. customto collect the crystals
9. filtrationby filtration
10. customThe crystals obtained
11. customwere recrystallized from methylene chloride