P(Cl)(Cl)([Cl:3])=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([S:13]([O-])(=[O:15])=[O:14])=[CH:9][C:8]=1[N+:17]([O-:19])=[O:18].[K+].C(#N)C.CC(N(C)C)=O>O>[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([S:13]([Cl:3])(=[O:15])=[O:14])=[CH:9][C:8]=1[N+:17]([O-:19])=[O:18]1250 ml of phosphorus oxychloride was added dropwise to a mixture comprising 1280 g of potassium 4-chloro-3-nitrobenzenesulfonate, 1150 ml of acetonitrile, 250 ml of sulforane and 30 ml of dimethylacetamide, while the inner temperature of the reaction system was kept at from 60° C. to 70° C. After being reacted for 3 hours at 73° C., the reaction mixture was cooled with water and 400 ml of water was gradually added thereto, and then the resulting mixture was poured into 5 liters of ice-water. The crystal precipitated was taken out by filtration, washed with water and dried. Yield: 1060 g, 84%.
読み込み中…
