C([O:3][CH:4](OCC)[CH2:5][N:6]([CH2:9][CH3:10])[CH2:7][CH3:8])C.Cl.[OH:15][S:16]([O-:18])=[O:17].[Na+:19].C(O)C>O>[CH2:7]([N:6]([CH2:9][CH3:10])[CH2:5][CH:4]([OH:3])[S:16]([O-:18])(=[O:17])=[O:15])[CH3:8].[Na+:19]2,2-diethoxy-N,N-diethylethanamine (140 mg, 0.75 mmol) was added in 0.1 mL H2O. Concentrated HCl (190 mg) was added dropwise in an ice bath. The solution was stirred for 2 hours at 40 degree. NaHSO3 (350 mg, 3.36 mmol) in 0.6 mL H2O was added to the reaction solution in an ice bath and stirred for 1 hour at room temperature, then 0.6 ml ethanol was added and stirred for 1 hour at room temperature. This reaction solution was concentrated, the resulting residue was used directly for the next step.
Wird geladen…
