反应详情

20 Grams of o-methoxycarbonyl- -[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide, 400 ml of methanol and 25 ml of 3.5N-potassium hydroxide methanol solution were mixed together and the mixture was refluxed for 8.5 hours. After completion of the reaction, the reaction mixture was allowed to stand for cooling, then an ethanol solution of hydrochloric acid was added to the mixture to adjust the pH thereof to about 1. The crystals formed were removed by filtration, and the mother liquor was cooled by ice. The crystals were collected by filtration, recrystallized from 80% water-containing methanol to obtain 13.28 g of o-carboxy- -[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide monohydrochloride in the form of colorless cotton fiber-like crystals. Melting point: 250.5°-251.5° C. (decomposed).

1. temperaturethe mixture was refluxed for 8.5 hours
2. customAfter completion of the reaction
3. temperaturefor cooling
4. customThe crystals formed
5. customwere removed by filtration
6. temperaturethe mother liquor was cooled by ice
7. filtrationThe crystals were collected by filtration
8. customrecrystallized from 80% water-
9. additioncontaining methanol