Nitrobenzene → 3-Nitrobenzenesulfonyl chloride

Participants

Reaction Conditions

Reaction Steps

Chlorosulfonic acid (475 g) was taken in a 1 L three neck round bottom flask equipped with a guard tube and liquid addition funnel. Chlorosulfonic acid was cooled in an ice bath to 5-10° C. and nitrobenzene was added to the acid slowly, at such a rate that the temperature is maintained below 10° C. Reaction mixture was then brought to 25° C. and then slowly heated in an oil bath to 80-85° C. Reaction mixture was stirred further at 80-85° C. for 3 hours. After the completion of reaction (TLC), the reaction mixture was cooled to 10° C. and poured onto the ice-water mixture along with stirring and maintaining the temperature below 10° C.; the resulting slurry is then filtered on buchner funnel. Solid cake on funnel is washed with 500 mL of water. Resulting solid cake is dried on phosphorous pentoxide in a desiccator to obtain the D1 as off white solid.

Provenance & Evidence