Ammonium Chloride → HCID 57642245, compound

Participants

Reaction Conditions

Reaction Steps

Sodium borohydride (5 mg, 0.13 mmol) was added to an ice-cooled solution of 3-{2-[5-cyclohexyl-1-(3,3-dimethyl-2-oxo-butyl)-2-oxo-1,2-dihydro-3H-1,3,4-benzotriazepin-3-yl]-acetylamino}-5-methylamino-benzoic acid methyl ester (Example 74)(64 mg, 0.11 mmol) in MeOH (2 ml). The reaction mixture was stirred at 0-5° C. for 40 mins, then at room temperature for 2 h. Saturated NH4Cl solution (10 ml) was added and the product was extracted with CHCl3 (15 ml). The organic phase was dried (MgSO4), filtered and the filtrate was evaporated to afford the title compound (60 mg, 97%). 1H NMR (CDCl3) 8.10-8.79 (1H, m), 7.55 (2H, m), 7.36 (2H, m), 7.24 (1H, m), 6.95 (1H, s), 6.70 (1H, m), 4.46 (1H, m), 4.29-4.04 (2H, m), 3.89 (4H, m), 3.82-3.60 (1H, m), 3.43-3.23 (1H, m), 2.81 (4H, m), 2.15-1.66 (7H, m), 1.33-1.24 (3H, m), 0.97 and 0.93 (9H, s×2). Found C, 63.17; H, 7.59; N, 11.85%; C31H41N5O5.1.5H2O requires C, 63.03, H, 7.51, N 11.86%.

Provenance & Evidence