反应详情

Concentrated hydrochloric acid (1 ml) was added to a suspension of 4-[(3-bromo-2-(2-(2-triphenylmethyl-2H-tetrazol-5-yl)phenyl)benzofuran-5-yl)methoxy]-2-ethyl-5,6,7,8-tetrahydroquinoline (A) (650 mg) in methanol (2 ml) and ethanol (4 ml). The mixture was warmed gently until the solid dissolved and then left to stand for 2 hours. The precipitated solid was filtered off, slurried with ether (10 ml) and recrystallised from methanol to give 4-[(3-bromo-2-(2-(1H-tetrazol-5-yl)phenyl)benzofuran-5-yl)methoxy]-2-ethyl-5,6,7,8-tetrahydroquinoline hydrochloride, m.p. 210°-212° C.; NMR (d6 -DMSO): 1.3(t, 3H), 1.65-1.9(m, 4H), 2.5-2.7(m, 2H), 2.9-3.1(m, 4H), 5.6(s, 2H), 7.55(s, 1H), 7.6(s, 2H), 7.7(s, 1H), 7.75-7.85(m, 2H), 7.9-8.0(m, H); mass spectrum (+ve fast atom bombardment (+FAB), DMSO/Methanol/nitrobenzyl alcohol(NBA)): 532 (M+H)+ ; microanalysis, found: C, 57.0; H, 4.6; N, 12.4%; C27H24BrN5O2.HCl requires: C, 57.2; H, 4.45; N, 12.4%.

1. temperatureThe mixture was warmed gently until the solid
2. dissolutiondissolved
3. waitleft
4. filtrationThe precipitated solid was filtered off
5. customrecrystallised from methanol