Hydrochloric Acid → HCID 69021592, compound

Participants

Reaction Conditions

Reaction Steps

Intermediate (30) (0.01125 mol) was cooled on an ice bath. Hydrochloric acid (90 ml) was added. Then a solution of sodium nitrite (0.013 mol) in water (18 ml) was added quickly dropwise. The mixture was stirred at 5° C. for 30 min and at room temperature for 2 hours. Water was added. The mixture was basified with K2CO3 10% and extracted with DCM. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated till dryness. The residue (6 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 90/10; 15–40 μm). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from DCM/DIPE. The precipitate was filtered off and dried, yielding 1 g (19.6%) of (4-chlorophenyl)[6-(3-chlorophenyl)-4H,6H-tetrazolo[1,5-a][4,1]benzothiazepin-8-yl]-methanone (intermediate 31), mp. 212° C.

Provenance & Evidence