[Cl:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][C:10](=[O:19])[C:11](=[N:17]O)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:5]=[CH:6][CH:7]=1.O.[C:21](O)(=[O:23])[CH3:22]>C(OC(=O)C)(=O)C.[Zn]>[C:21]([NH:17][CH:11]([C:10](=[O:19])[CH2:9][CH2:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13])(=[O:23])[CH3:22]To a stirred solution of the product from step (ii) in acetic acid (125 ml) and acetic anhydride (40 ml) was added zinc dust (45 g) portionwise at a rate to maintain the internal temperature <40° C. The mixture was stirred for 30 min and water (125 ml) was added at such a rate as to maintain the temperature at around 40° C. The mixture was stirred at room temperature for 2 hours and filtered. The mother liquor was extracted with dichloromethane and further washed with water. The organic layer was collected, dried (MgSO4) and solvent evaporated under reduced pressure to give the subtitle product.
Wird geladen…
