[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:17])[C:9]2[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[CH3:18]OP(C(=[N+]=[N-])C(=O)C)(=O)OC.C([O-])([O-])=O.[K+].[K+]>CO>[C:13]([C:12]1[CH:15]=[CH:16][C:9]([CH:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[OH:17])=[CH:10][CH:11]=1)#[CH:18]A mixture of the product of Step B (0.21 g, 0.91 mmol), dimethyl(1-diazo-2-oxopropyl)phosphonate (0.21 g, 1.1 mmol) and K2CO3 (0.152 g, 1.1 mmol) in anhydrous MeOH (5 ml) was stirred for overnight at room temperature. The solvent was distilled off and the residue was taken in EtOAc (50 ml), washed with H2O and dried over MgSO4 and filtered. The filtrate was evaporated under reduced pressure to give the crude product (0.195 g; 95%), which was used in the next step without purification. 1H-NMR (CDCl3) 3.05 (s, 1H); 5.76 (s, 1H); 7.0 (tr, 2H, J=8.58 Hz); 7.25-7.33 (m, 4H); 7.44 (d, 2H, J=8.29 Hz).
Wird geladen…
