反应详情

A mixture of the compound 111 (306 mg, 0.7 mmol), dibenzylamine (138 mg, 0.7 mmol) and paraformaldehyde (22.0 mg., 0.733 mmol) in ethyl acetate (4 mL) was heated under reflux in an atmosphere of nitrogen for 8 hours. After cooling down at room temperature, the reaction mixture was purified by chromatography on a silica gel column (eluate: ethyl acetate) to give the compound 114 (295 mg, 64%). Rf 0.70 (EtOAc). 1H-NMR (CDCl3): δH1.31 (6 H, d, J 6.6 Hz, (CH3)2CH), 3.18 (1 H, sep, J 6.6 Hz, (CH3)2CH), 3.57 (4H, s, 2 x benzyl-CH2), 4.04 (2 H, d, J 6.0 Hz, NCH2NH), 4.88 (1H, t, 6.0 Hz, NCH2NH), 5.19 (2 H, s, CH2O), 5.24 (2 H, s, NCH2), 6.68 (2 H, d, J 1.5 Hz, arom 2- and 6-H), 6.78 (2 H, d-like, 4-pyridyl 2- and 6-H), 7.03 (1 H, t, J 1.5 Hz, arom 4-H), 7.20-7.35 (10 H, m, 2 x benzyl), 8.43 (2 H, d-like, 4-pyridyl 3- and 5-H). Elementary analysis (for C35H35N5O2SCl2) Calcd.: C, 63.63% H, 5.34% N, 10.60% S, 4.85% Cl, 10.73% Found: C, 63.39% H, 5.44% N, 10.63% S, 4.88% Cl, 10.53% The above compounds are shown as follows. ##STR6##

1. temperaturewas heated
2. temperatureunder reflux in an atmosphere of nitrogen for 8 hours
3. customthe reaction mixture was purified by chromatography on a silica gel column (eluate: ethyl acetate)