[CH3:1][NH:2][CH3:3].Cl.[CH3:5][N:6]([CH2:8][C:9]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:14][CH2:13][C:12](=O)[CH2:11][CH2:10]1)[CH3:7].[C-:22]#[N:23].[K+]>O.CO>[CH3:1][N:2]([CH3:3])[C:12]1([C:22]#[N:23])[CH2:13][CH2:14][C:9]([CH2:8][N:6]([CH3:7])[CH3:5])([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:10][CH2:11]140% aqueous dimethylamine solution (12.8 mL, 21.1 mmol) was added in drops to a mixture of 4N hydrochloric acid (5 mL) and methanol (3 mL) with ice cooling. The title compound of step 6 (4.89 g, 21.1 mmol) and KCN (3.30 g, 50.7 mmol) were then added one after the other. The mixture was stirred for 3 d at RT. For work up the batch was mixed with water (10 mL) and extracted with diethyl ether (3×20 mL). The ether phase was concentrated to low volume in a vacuum, the residue was taken up in CH2Cl2, dried over Na2SO4 and concentrated to low volume in a vacuum.
Wird geladen…
