O/[N:2]=[C:3]1/[C:4](=O)[C:5]2[C:10]([CH2:11]/1)=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[CH:6]=2.P(Cl)(Cl)(Cl)(Cl)[Cl:16].[ClH:21]>O=P(Cl)(Cl)Cl>[Cl:21][C:4]1[C:5]2[C:10](=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[CH:6]=2)[CH:11]=[C:3]([Cl:16])[N:2]=1To a suspension of (E)-2-(hydroxyimino)-6-methoxy-2,3-dihydro-1H-inden-1-one (3.60 g, 20.0 mmol) in POCl3 (120 mL), PCl5 (6.50 g, 31.3 mmol) was added at 0° C., then HCl gas was induced until the solution was saturated. The reaction mixture was stirred at 30° C. for 2 hours. The solvent was removed in vacuo and ice water was added to the residue. The precipitate was collected by filtration, washed with water (30 mL), and dried under high vacuum to give the product (4.50 g, yield 85%) as a solid.
Wird geladen…
