[CH:1]1[CH:6]=[CH:5][C:4]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=2)=[CH:3][CH:2]=1.N1C=CC=CC=1.[Cl:21][C:22](Cl)([O:24]C(=O)OC(Cl)(Cl)Cl)Cl>C(Cl)Cl>[Cl:14][C:10]1[CH:9]=[C:8]([N:7]([C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)[C:22]([Cl:21])=[O:24])[CH:13]=[CH:12][CH:11]=1To a solution of 3-chlorodiphenylamine (3.0 g) and pyridine (1.43 mL) in CH2Cl2 (30 mL) was added triphosgene (1.75 g) at 5° C. After stirring at room temperature for 6 hours, the mixture was evaporated, diluted with EtOAc, washed with water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane-EtOAc 15:1) to give N-(3-chlorophenyl)-N-phenylcarbamoyl chloride (4.05 g) as an oil.
Wird geladen…