[CH3:1][C:2]([CH3:29])([O:4][C:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][C:20](=[O:28])[C:21]3[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=3)=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)=[O:6])[CH3:3].C([O-])([O-])=O.[Cs+].[Cs+].Br[CH2:37][C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39]>CCOC(C)=O>[CH3:3][C:2]([CH3:29])([O:4][C:5]([N:7]1[CH2:8][CH2:9][N:10]([C:13]2[CH:14]=[CH:15][C:16]([NH:19][C:20]([C:21]3[CH:22]=[CH:23][C:24]([O:27][CH2:37][C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39])=[CH:25][CH:26]=3)=[O:28])=[CH:17][CH:18]=2)[CH2:11][CH2:12]1)=[O:6])[CH3:1]To a 100 mL round bottomed flask with a stirring bar and an argon inlet was added N-(4-(4-(1,1-dimethylethoxycarbonyl)piperazin-1-yl)phenyl)-4-hydroxybenzamide (0.56 g, 1.41 mmol) DMF (35 mL), Cs2CO3 (0.49 g, 1.51 nmmol) and tert-butyl bromoacetate (0.28 mL, 1.75 mmol). This mixture was stirred at ambient temperature for 18 h. The mixture was diluted with EtOAc and washed with H2O and brine. Drying (MgSO4), filtration and removal of the solvent in vacuo gave 0.78 g of tert-butyl 4-(4-(4-(1,1-dimethylethoxycarbonyl)piperazin-1-yl)phenylaminocarbonyl)phenoxyacetate which was used in the next step without purification.
Wird geladen…