Acetonitrile → Benzenesulfonyl chloride, 4-chloro-3-nitro-

Participants

Reaction Steps

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%.

Provenance & Evidence