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

Participants

Reaction Steps

To a mixture of 1280 g of potassium 4-chloro-3-nitrobenzenesulfonate, 1150 ml of acetonitrile, 250 ml of sulforan, and 30 ml of dimethylacetamide was added dropwise 1250 ml of phosphorus oxychloride so that the internal temperature was kept at 60° C. to 70° C. Then, after performing the reaction for 3 hours at 73° C., the reaction mixture was cooled with water and after adding slowly 400 ml of water thereto, the mixture was poured into 5 liters of ice-water. Crystals thus deposited were recovered by filtration, washed, and dried to provide 1060 g of the above-described compound with a yield of 84%. The melting point thereof was 55° C. to 56° C.

Provenance & Evidence