[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([O-])(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[K+].P(Cl)(Cl)([Cl:18])=O.O>C(#N)C.S1(CCCC1)(=O)=O.CC(N(C)C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([Cl:18])(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13]To a solution mixture of 1,280 g of potassium 4-chloro-3-nitrobenzenesulfonate in 1,150 ml of acetonitrile, 250 ml of sulfolane and 30 ml of dimethylacetamide was added dropwise 1,250 ml of phosphorus oxychloride while the temperature was kept at 60° to 70° C. After the reaction proceeded for 3 hours at 73° C., the reaction mixture was cooled with water, then 400 ml of water was added thereto gradually, and then 5 liters of ice water was poured into the reaction mixture. The deposited crystals were filtered followed by washing with water and drying.
불러오는 중…
