反应详情

8.28 Grams of potassium carbonate was dissolved in 50 ml of water-acetone (1:2), and to this solution was added 15.1 g of o-methoxycarbonylaniline. Under ice-cooled condition, an acetone solution of 34.4 g of [4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetylchloride was added dropwise thereto. After completion of the addition, the reaction was carried out at a room temperature for 3 hours, then acetone was removed by distillation. The residue obtained was extracted with chloroform, then the extract was washed with water, dried and chloroform was removed by distillation. The residue obtained was crystallized by adding ethyl acetate, and the crystals were collected by filtration. Recrystallized from ethanol to obtain 29 g o-methoxycarbonyl-α-[4-3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide in the form of colorless needle-like crystals. Melting point: 167.5°-169.0° C.

1. temperatureUnder ice-cooled condition
2. additionAfter completion of the addition
3. customacetone was removed by distillation
4. customThe residue obtained
5. extractionwas extracted with chloroform
6. washthe extract was washed with water
7. customdried
8. customchloroform was removed by distillation
9. customThe residue obtained
10. customwas crystallized
11. additionby adding ethyl acetate
12. filtrationthe crystals were collected by filtration
13. customRecrystallized from ethanol