反应详情

A solution of 56.9 parts of 1-[5,5-bis(4-fluorophenyl)-4-pentenyl]-4-(phenylmethyl)-2-piperazinecarboxamide in 400 parts of methanol was hydrogenated in a Parr apparatus and at 50° C. with 5 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated in vacuo. The residue was dissolved in 2-propanone and the whole was acidified with a mixture of hydrochloric acid and 2-propanol. After the addition of 2,2'-oxybispropane, the supernatant liquid was decanted and the precipitate was stirred in 2,2'-oxybispropane. The precipitated product was filtered off and dissolved in water. After washing with 2,2'-oxybispropane, the aqueous layer was treated with ammonium hydroxide and the product was extracted with trichloromethane. The extract was washed with a sodium chloride solution, dried, filtered and evaporated (under trichloromethane), yielding 35.2 parts (76.3%) of 1-[5,5-bis(4-fluorophenyl)pentyl]-2-piperazinecarboxamide as a residue (int. 34).

1. filtrationthe catalyst was filtered off
2. customthe filtrate was evaporated in vacuo
3. dissolutionThe residue was dissolved in 2-propanone
4. additionthe whole was acidified with a mixture of hydrochloric acid and 2-propanol
5. additionAfter the addition of 2,2'-oxybispropane
6. customthe supernatant liquid was decanted
7. filtrationThe precipitated product was filtered off
8. dissolutiondissolved in water
9. washAfter washing with 2,2'-oxybispropane
10. additionthe aqueous layer was treated with ammonium hydroxide
11. extractionthe product was extracted with trichloromethane
12. washThe extract was washed with a sodium chloride solution
13. customdried
14. filtrationfiltered
15. customevaporated (under trichloromethane)