[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:18])[NH:10][C:11]([CH3:17])([CH3:16])[C:12](OC)=[O:13])=[CH:4][C:3]=1[C:19]1[S:20][CH:21]=[CH:22][CH:23]=1.Cl>O1CCCC1.C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([CH3:17])([CH3:16])[NH:10][C:9]2=[O:18])=[CH:4][C:3]=1[C:19]1[S:20][CH:21]=[CH:22][CH:23]=10.62 g of compound 267.3 was dissolved at room temperature in 5 ml of dry tetrahydrofuran, admixed with 0.62 ml of concentrated hydrochloric acid and stirred at 80° C. for 2 h. The cooled reaction mixture was taken up in ethyl acetate and washed with saturated sodium hydrogencarbonate solution, and the organic phase was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was stirred with diisopropyl ether, filtered and dried. 3-(4-Fluoro-3-thiophen-2-yl-phenyl)-5,5-dimethylimidazolidine-2,4-dione (267.2) was obtained. Molecular weight 304.06 (C15H13FN2O2S); retention time Rt=2.25 min. [E]; MS (ESI): 346.09 (MH++CH3CN).
Loading…