C(O)C.[C-:4]#[N:5].[Na+].CS(O[CH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]1[N:18]([CH3:20])[CH3:19])(=O)=O.C(=O)([O-])[O-].[Na+].[Na+]>Cl.C(Cl)Cl>[CH3:19][N:18]([CH3:20])[CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH:12]1[C:4]#[N:5]To 200 mL of 80% aqueous ethanol add 10 g (0.2 mol) of sodium cyanide and 22.1 (0.1 mol) of 2-(dimethylamino)-cyclohexanol methanesulfonate. Reflux the reaction and monitor by thin-layer chromatography. Upon completion add in HCl until gas evolution ceases. Remove solvent in vacuo and add saturated aqueous sodium carbonate (ph=11) and 100 mL of methylene chloride. Separate the layers and dry the organic phase over Na2SO4. Filter the drying agent and evaporate the solvent in vacuo to obtain the title compound.
Wird geladen…
