反应详情

8.28 Grams of potassium carbonate was dissolved in 50 ml of water-acetone (1:2), then 13.6 g of o-carbamoylaniline was added thereto. Under ice-cooled condition, an acetone solution of 34.4 g of [4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetyl chloride was added dropwise to the said mixture, then the reaction was carried out at a room temperature for 3 hours. Acetone was removed by distillation, the residue obtained was extracted with chloroform and the extract was washed with water, dried then chloroform was removed by distillation. The residue obtained was purified by a silica gel column chromatography, the product obtained was converted into a hydrochloride by adding hydrochloric acid-ethanol, recrystallized from water-acetone to obtain 16 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. temperatureUnder ice-cooled condition
2. customAcetone was removed by distillation
3. customthe residue obtained
4. extractionwas extracted with chloroform
5. washthe extract was washed with water
6. customdried
7. customchloroform was removed by distillation
8. customThe residue obtained
9. customwas purified by a silica gel column chromatography
10. customthe product obtained
11. customrecrystallized from water-acetone