Water → 1-Naphthalenesulfonyl chloride

Participants

Reaction Conditions

Reaction Steps

133 g of sodium α-naphthalenesulfonate was suspended in a mixture of 260 ml of acetonitrile and 7 ml of dimethylacetamide. 80 ml of phosphorus oxychloride was added dropwise to the suspension while being cooled with water at a temperature of lower than 50° C. After the dropwise addition was completed, the reaction system was further reacted at a temperature of 65° C. for 1 hour. After cooled to 30° C., the reaction mixture was poured into 2 l of ice water. The resulting grayish white crystal was filtered off, and air-dried. The yield was 110.8 g (84.6% of theoretical value). The melting point of the product was 66° to 68° C.

Provenance & Evidence