[ClH:1].[CH2:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:17][CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]1)[CH3:3]>CCOC(C)=O>[ClH:1].[CH2:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)[CH3:3]Excess HCl in EtOAc was added dropwise to a solution of intermediate 30 (800 mg, 2.5 mmol) in EtOAc and the reaction mixture was stirred at rt for 1.5 h. Filtration gave 1-(2-ethoxyphenyl)-1,4-diazepane hydrochloride (intermediate 31) (382 mg, 59%) as a white solid.
Wird geladen…