反应详情

Concentrated hydrochloric acid (0.3 ml) was added to a solution of 5,7-dimethyl-1-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methyl]-1,6-naphthyridin-2(1H)-one (280 mg) (A) in dichloromethane/methanol (4 ml) (3:1 v/v) and the mixture was stirred for 30 minutes. Volatile material was removed by evaporation and the residue was stirred with ether. The insoluble solid was collected by filtration and recrystallised from ethanol/methanol (1:1 v/v) to give 5,7-dimethyl-1-[(2'-(1H-tetrazol-5-yl)biphenyl-4-yl)methyl]-1,6-naphthyridin-2(1H)-one hydrochloride (105 mg), as a solid, m.p. 278°-280° C. (decomposition); NMR (d6 -DMSO): 2.68(s,3H), 2.96(s,3H), 5.51(s,2H), 6.94(d,1H), 7.05(d,2H), 7.17(d,2H), 7.45-7.71(m,5H), 8.31(d,1H); mass spectrum (positive fast atom bombardment (+ve FAB), DMSO/methanol/nitrobenzyl alcohol(NBA)): 409(M+H)+ ; microanalysis, found: C, 64.1; H, 4.6; N, 18.7%; C24H20N6O.HCl.0.2H2O requires: C,64.1; H,4.8; N,18.7%.

1. customVolatile material was removed by evaporation
2. stirringthe residue was stirred with ether
3. filtrationThe insoluble solid was collected by filtration
4. customrecrystallised from ethanol/methanol (1:1 v/v)