反应详情

Sodium hydroborate (0.0005 mol) was added portionwise at room temperature to a mixture of intermediate 27 (0.0005 mol) in methanol (2.5 ml). The mixture was stirred at room temperature for 2 hours and poured out into ice water. DCM was added. The mixture was extracted with DCM. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified by column chromatography over kromasil® (5 μm) (eluent: DCM/MeOH/Et3N 97/3/0.3). The pure fractions were collected and the solvent was evaporated. The residue (0.1 g, 40%) was taken up in diethyl ether and dried in a vacuo, yielding 0.07 g (28%) of 5-(3-chlorophenyl)-4,5-dihydro-α-(1-methyl-1H-imidazol-5-yl)-α-(4-methylphenyl)-tetrazolo[1,5-a]quinazoline-7-methanamine (intermediate 28), mp. 140° C.

1. extractionThe mixture was extracted with DCM
2. customThe organic layer was separated
3. washwashed with water
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was purified by column chromatography over kromasil® (5 μm) (eluent: DCM/MeOH/Et3N 97/3/0.3)
8. customThe pure fractions were collected
9. customthe solvent was evaporated
10. customdried in a vacuo