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.S1(CCCC1)(=O)=O>O.CC(N(C)C)=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]
1,250 ml of phosphorus oxychloride was added dropwise to a mixture of 1,280 g of potassium 4-chloro-3-nitrobenzenesulfonate, 1,150 ml of acetonitrile, 250 ml of sulfolane, and 30 ml of dimethylacetamide in such a manner that the internal temperature thereof was kept at 60° to 70° C. After being allowed to react at a temperature of 73° C. for 3 hours, the reaction mixture was cooled with water, and 400 ml of water was gradually added to the reaction mixture. The cooled reaction mixture was then added to 5 l of ice water. The resulting crystals were filtered off, washed with water, and then dried. (Yield: 1,060 g (84%); m.p.: 55°-56° C.)
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