反应详情

5 Grams of methyl m-(α-chloroacetylamino)benzoate, 7.56 g of N-(3,4-dimethoxybenzoyl)piperazine monohydrochloride, 7.76 g of triethylamine and 30 ml of acetonitrile were mixed together and reacted at 45° to 50° C. for 5 hours. After completion of the reaction, the reaction mixture was ice-cooled, and the crystals formed were removed by filtration. The mother liquor was concentrated to dryness, and extracted by adding 1 N-sodium hydroxide aqueous solution and chloroform. The chloroform layer was washed with water, dried and removed by distillation. The oily substance obtained was purified by a silica gel column chromatography to obtain 10.08 g of m-methoxycarbonyl-α-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide in the form of colorless oily substance.

1. customreacted at 45° to 50° C. for 5 hours
2. customAfter completion of the reaction
3. temperaturecooled
4. customthe crystals formed
5. customwere removed by filtration
6. concentrationThe mother liquor was concentrated to dryness
7. extractionextracted
8. additionby adding 1 N-sodium hydroxide aqueous solution and chloroform
9. washThe chloroform layer was washed with water
10. customdried
11. customremoved by distillation
12. customThe oily substance obtained
13. customwas purified by a silica gel column chromatography