2-[(2-chloroacetyl)amino]benzamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 40 Grams of o-carbamoyl-α-chloroacetanilide, 40 g of benzylpiperazine, 52.4 ml of triethylamine and 250 ml of acetonitrile were heated at 50° C. for 5 hours with stirring, and crystals formed were collected by filtration. The crystals collected were extracted with chloroform and 1 N-sodium hydroxide aqueous solution, the chloroform layer was washed with water, dried then chloroform was removed by distillation. To the residue obtained was added ethanol and insoluble material formed was collected by filtration. Then the insoluble material was suspended in ethanol and was added hydrochloric acid/ethanol to make the pH of the mixture to about 1, then the solvent was removed by distillation. The residue obtained was crystallized by adding acetone, and recrystallized from methanol to obtain 54 g of o-carbamoyl-α-(4-benzyl-1-piperazinyl)acetanilide dihydrochloride. Colorless powdery crystals. Melting point: 218.5°-219.5° C. (decomposed). crystals formed were collected by filtration The crystals collected were extracted with chloroform and 1 N-sodium hydroxide aqueous solution the chloroform layer was washed with water dried chloroform was removed by distillation To the residue obtained formed was collected by filtration was added hydrochloric acid/ethanol the solvent was removed by distillation The residue obtained was crystallized by adding acetone recrystallized from methanol

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.00 Grams of o-carbamoyl-α-chloroacetanilide, 8.09 g of 3,4-dimethoxybenzoylpiperazine monohydrochloride, 8.31 g of triethylamine and 30 g of acetonitrile were mixed together and the mixture was stirred at 50° C. for 5 hours. Then the reaction mixture was ice-cooled, and the crystals formed were removed by filtration and the filtrate obtained was concentrated to dryness. The residue obtained was extracted with chloroform--1N sodium hydroxide aqueous solution, and the chloroform layer was washed with water, dried then chloroform was removed by distillation. The residue obtained was purified by a silica gel column chromatography and the desired product was converted into a hydrochloride by using hydrochloric acid-ethanol, then recrystallized from water-acetone to obtain 7.43 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). cooled the crystals formed were removed by filtration the filtrate obtained was concentrated to dryness The residue obtained was extracted with chloroform--1N sodium hydroxide aqueous solution the chloroform layer was washed with water dried chloroform was removed by distillation The residue obtained was purified by a silica gel column chromatography recrystallized from water-acetone