反应详情

6.15 Grams of o-carbamoyl-α-(1-piperazinyl)acetanilide and 2.4 g of triethylamine were dissolved in 50 ml of methylene chloride, then to this solution was added dropwise a methylene chloride solution of 5.4 g of 3,4-dimethoxybenzoyl chloride under ice-cooled condition with stirring. The reaction was carried out at the same temperature for 1 hour, then the reaction mixture was washed with water, 5%-sodium bicarbonate aqueous solution, and an aqueous solution of potassium carbonate, then dried. Methylene chloride was removed by distillation, the residue was purified by a silica gel column chromatography, the product obtained was converted into a hydrochloride by adding hydrochloric acid-ethanol, then recrystallized from water-acetone to obtain 5.1 g of o-carbamoyl-α-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide monohydrochloride monohydrate in the form of colorless needle-like crystals. Melting point: 122.0°-125.0° C. (decomposed).

1. temperaturecooled condition
2. washthe reaction mixture was washed with water, 5%-sodium bicarbonate aqueous solution
3. dry with materialan aqueous solution of potassium carbonate, then dried
4. customMethylene chloride was removed by distillation
5. customthe residue was purified by a silica gel column chromatography
6. customthe product obtained
7. customrecrystallized from water-acetone