反应详情

A mixture of intermediate 9 (0.0014 mol) in toluene (10 ml) was stirred and refluxed for 48 hours, then brought to room temperature and the solvent was evaporated till dryness. The residue was taken up in DCM. The solvent was evaporated till dryness. The residue was purified by column chromatography over kromasil® (10 μm) (eluent: DCM/MeOH/Et3N 95/5/0.1). The pure fractions were collected and the solvent was evaporated. The residue (0.4 g, 57%) was washed with diethyl ether. The precipitate was filtered off and dried under a vacuo, yielding 0.35 g (50%) of 9-(3-chlorophenyl)-α-(4-fluorophenyl)-4,9-dihydro-α-(1-methyl-1H-imidazol-5-yl)-tetrazolo[5,1-b]quinazoline-7-methanol (compound 2), mp. 180° C.

1. temperaturerefluxed for 48 hours
2. custombrought to room temperature
3. customthe solvent was evaporated till dryness
4. customThe solvent was evaporated till dryness
5. customThe residue was purified by column chromatography over kromasil® (10 μm) (eluent: DCM/MeOH/Et3N 95/5/0.1)
6. customThe pure fractions were collected
7. customthe solvent was evaporated
8. washThe residue (0.4 g, 57%) was washed with diethyl ether
9. filtrationThe precipitate was filtered off
10. customdried under a vacuo