反应详情

A mixture of (±)-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-2-(1-methyl-2-oxopropyl)-3H-1,2,4-triazol-3-one (0.018 mol), (S)-α-methyl-1-naphthalenemethanamine (0.0187 mol) and sodium tris(acetato-O)hydroborate (I-) (0.028 mol) in CH2Cl2 (150 ml) was stirred at room temperature overnight. A diluted NH4OH solution was added. The mixture was stirred for 1 hour. The precipitate was filtered off, washed with H2O and with CH2Cl2 (20 ml) and dried. The residue was crystallized from CH3CN. The precipitate was filtered off and dried, yielding 3.3 g (32%) of [R-(R*,S*)(S*)]-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-2-[1-metyl-2-[[1-(1-naphthalenyl)ethyl]amino]propyl]-3H-1,2,4-triazol-3-one (interm. 108).

1. stirringThe mixture was stirred for 1 hour
2. filtrationThe precipitate was filtered off
3. washwashed with H2O and with CH2Cl2 (20 ml)
4. customdried
5. customThe residue was crystallized from CH3CN
6. filtrationThe precipitate was filtered off
7. customdried