[CH3:1][O:2][C:3](=[O:16])[C:4](=O)[CH:5](Cl)[CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[NH2:17][C:18]([NH2:20])=[S:19].N.CO>CO.[Cl-].[Na+].O>[CH3:1][O:2][C:3]([C:4]1[N:17]=[C:18]([NH2:20])[S:19][C:5]=1[CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:16]Reflux equimolar 3-chloro-2-oxo-5-phenyl-pentanoic acid methyl ester and thiourea in MeOH (1.0 M) for 4 h. Basify with ammonia-MeOH and add brine. Extract with ethyl acetate (4×). Wash combined organic layers with brine, dry (MgSO4), and concentrate under reduced pressure to give (91%) of title compound. HPLC (GRAD80-100M) t=2.193 (95%). MS (APCI): 263 (M+1).
Wird geladen…