反应详情

A mixture of intermediate (5) (0.19 mole) in methanol (600 ml) and THF (600 ml) was hydrogenated overnight with Pd/C 10% (3 g) as a catalyst. After uptake of hydrogen (1 equivalent), the catalyst was filtered off and the filtrate was evaporated. The residue was triturated in DIPE. The precipitate was filtered off, dried, and dissolved in water. The mixture was alkalinized with Na2CO3 and then extracted with DCM. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was triturated in DIPE. The precipitate was filtered off and dried, yielding 40 g of N-[4-(1-piperazinyl)phenyl]-4′-(trifluoromethyl)-[1,1′-biphenyl]-2-carboxamide (intermediate 6).

1. customthe filtrate was evaporated
2. customThe residue was triturated in DIPE
3. filtrationThe precipitate was filtered off
4. customdried
5. dissolutiondissolved in water
6. extractionextracted with DCM
7. customThe organic layer was separated
8. customdried
9. filtrationfiltered
10. customthe solvent was evaporated
11. customThe residue was triturated in DIPE
12. filtrationThe precipitate was filtered off
13. customdried