[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][C:5]=2[CH:4]=1.C(N(CC)CC)C.[CH3:28][NH:29][CH2:30][CH2:31][CH2:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[C:35]([O:41][CH3:42])[CH:34]=1>C(Cl)Cl.O.CC(C)=O>[ClH:15].[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][N:29]([CH3:28])[CH2:30][CH2:31][CH2:32][C:33]3[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[C:35]([O:41][CH3:42])[CH:34]=3)[CH2:10][CH2:11][C:5]=2[CH:4]=1A mixture of 5.55 gm (0.0186 mol) of 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-chloro-propane, 2.6 ml (0.0886 mol) of triethylamine and 3.9 gm (0.0186 mol) of N-methyl-3-(3,4-dimethoxy-phenyl) propylamine was heated at 85° C. for 4 hours, then cooled and dissolved in methylene chloride/water. The organic phase was separated, extracted with water, dried over magnesium sulfate, concentrated by evaporation in vacuo, and the residue was purified on silica gel, using methylene chloride plus 3% ethanol as the eluant. The oily free base product thus obtained was dissolved in acetone, and the hydrochloride was precipitated with ethereal hydrochloric acid.
Wird geladen…