반응 #63621

반응 방정식

hydrogen

thiophene

ethanol

4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethyl-4-nitrophenyl)-2-[(methylamino)carbonyl]-1-piperazineacetamide

→

N-(4-amino-2,6-dimethylphenyl)-4-[4,4-bis(4-fluorophenyl)butyl]-2-[(methylamino)carbonyl]-1-piperazineacetamide

용매

methanol

반응 조건

후처리

1. 1
   여과the catalyst was filtered off
2. 2
   기타the filtrate was evaporated
3. 3
   기타The residue was purified by column-chromatography over silica gel using
4. 4
   workup.ADDITIONa mixture of trichloromethane and methanol (95:5 by volume) as eluent
5. 5
   기타The pure fractions were collected
6. 6
   기타the eluent was evaporated

실험 절차

To 1 part of a solution of 2 parts of thiophene in 40 parts of ethanol were added 3 parts of 4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethyl-4-nitrophenyl)-2-[(methylamino)carbonyl]-1-piperazineacetamide and 120 parts of methanol. The whole was hydrogenated at normal pressure and at room temperature with 2 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. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was suspended in 2,2'-oxybispropane, yielding 2.14 parts of N-(4-amino-2,6-dimethylphenyl)-4-[4,4-bis(4-fluorophenyl)butyl]-2-[(methylamino)carbonyl]-1-piperazineacetamide; mp. 111.7° C. (compound 162).

출처