反应详情

温度

50 °C

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).

1. temperaturecooled
2. customthe crystals formed
3. customwere removed by filtration
4. customthe filtrate obtained
5. concentrationwas concentrated to dryness
6. customThe residue obtained
7. extractionwas extracted with chloroform--1N sodium hydroxide aqueous solution
8. washthe chloroform layer was washed with water
9. customdried
10. customchloroform was removed by distillation
11. customThe residue obtained
12. customwas purified by a silica gel column chromatography
13. customrecrystallized from water-acetone