C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[SH:14].Cl[CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[CH2:18].ClC=C(C1C=CC=CC=1)C>CC(C)=O.CCOCC.O>[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:14][CH2:18][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[CH2:16]
Potassium carbonate (4.6 g, 0.033 mole) is suspended in acetone (100 cc) and the whole is heated to 50°-60° C. An acetone (30 cc) solution of 2-chlorothiophenol (4.3 g, 0.03 mole) and of a mixture (9.1 g, 0.03 mole) containing 1-chloro-2-phenyl-2-propene (50%) and 1-chloro-2-phenyl-1-propene (50%) is added dropwise under nitrogen. After 1 h of stirring at 50°-60° C. the reaction mixture is poured into water and ice (150 g) and is then reextracted with ether (3×100 cc). It is washed with water (2×150 cc) and dried over MgSO4. The crude (11.7 g) is distilled in a ball oven to give 1-[2'-chlorophenylthio]-2-phenyl-2-propene (6.3 g, 80%) Bp0.5 =180° C. nD24 =1.6340.
Wird geladen…
