反应详情

A mixture of 4-[4-(phenylmethyl)-1-piperazinyl]-benzenamine (0.12 mole) in THF (300 ml) and triethylamine (50 ml) was stirred. [1,1′-Biphenyl]-2-carbonyl chloride (0.12 mole) was added dropwise. The mixture was stirred overnight. The solvent was evaporated. The residue was dissolved in DCM. The organic layer was separated, washed, dried, filtered and the solvent was evaporated. The residue was triturated in DIPE/2-propanol. The precipitate was filtered off and dried. A part (1 g) of this fraction was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 99/1). The pure fractions were collected and the solvent was evaporated. The residue was triturated in DIPE. The precipitate was filtered off and dried, yielding 0.84 g of N-[4-[4-(phenylmethyl)-1-piperazinyl]phenyl]-[1,1′-biphenyl]-2-carboxamide (intermediate 9, melting point 162° C.).

1. stirringThe mixture was stirred overnight
2. customThe solvent was evaporated
3. dissolutionThe residue was dissolved in DCM
4. customThe organic layer was separated
5. washwashed
6. customdried
7. filtrationfiltered
8. customthe solvent was evaporated
9. customThe residue was triturated in DIPE/2-propanol
10. filtrationThe precipitate was filtered off
11. customdried
12. customA part (1 g) of this fraction was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 99/1)
13. customThe pure fractions were collected
14. customthe solvent was evaporated
15. customThe residue was triturated in DIPE
16. filtrationThe precipitate was filtered off
17. customdried