反应详情

Raney nickel (6.5 g) was added to a solution of 5-(3-chlorophenyl)-α-(4-chlorophenyl)-α-[4-methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl)-tetrazolo[1,5-a]quinazoline-7-methanamine (0.0012 mol) in 2-propanone (30 ml) under N2 flow. The mixture was stirred at room temperature for 1 hour and 30 minutes, filtered over celite and rinsed with CH2Cl2/CH3OH. The solvent was evaporated. The residue was taken up in DCM. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated. The residue (0.4 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH; 96/4/0.5; 15–35 μm). The pure fractions were collected and the solvent was evaporated The residue was crystallized from CH3CN/diethyl ether. The precipitate was filtered off and dried, yielding 0.11 g (18%) of 5-(3-chlorophenyl)-α-(4-chlorophenyl)-α-(4-methyl-4H-1,2,4-triazol-3-yl)-tetrazolo[1,5-a]quinazoline-7-methanamine, mp. 220° C.

1. filtrationfiltered over celite
2. washrinsed with CH2Cl2/CH3OH
3. customThe solvent was evaporated
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe residue (0.4 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH; 96/4/0.5; 15–35 μm)
9. customThe pure fractions were collected
10. customthe solvent was evaporated The residue
11. customwas crystallized from CH3CN/diethyl ether
12. filtrationThe precipitate was filtered off
13. customdried