反应详情

2.5 Grams of [4-(4-methoxybenzoyl)-1-piperazinyl]acetic acid was dissolved in 30 ml of DMF, then 1.2 g of triethylamine was added thereto. Under an ice-cooled condition with stirring, 1.4 g of isobutyl chloroformate was added dropwise thereto and stirred for 30 minutes. Then, the reaction mixture was stirred at a room temperature, a DMF solution of 1.6 g of o-methoxycarbonylaniline was added dropwise to the reaction mixture and stirred for 6 hours. The reaction mixture obtained was concentrated to dryness, and the residue obtained was extracted with chloroform and 1 N-sodium hydroxide. The chloroform layer was washed with water, dried and then chloroform was removed by distillation. The residue obtained was crystallized by adding ethyl acetate, the crystals formed were collected by filtration. Recrystallized from ethanol to obtain 2.1 g of o-methoxycarbonyl-α-[4-(4-methoxybenzoyl)-1-piperazinyl]acetanilide in the form of colorless needle-like crystals. Melting point: 167.5°-169.0° C.

1. temperatureUnder an ice-cooled condition
2. stirringstirred for 30 minutes
3. stirringThen, the reaction mixture was stirred at a room temperature
4. stirringstirred for 6 hours
5. customThe reaction mixture obtained
6. concentrationwas concentrated to dryness
7. customthe residue obtained
8. extractionwas extracted with chloroform and 1 N-sodium hydroxide
9. washThe chloroform layer was washed with water
10. customdried
11. customchloroform was removed by distillation
12. customThe residue obtained
13. customwas crystallized
14. additionby adding ethyl acetate
15. customthe crystals formed
16. filtrationwere collected by filtration
17. customRecrystallized from ethanol