Chlorosulfonic acid → HCID 21555929, compound

Participants

Reaction Steps

6.6 ml (0.100 mol) of chlorosulphonic acid are cooled in an ice bath to 4°C whilst stirring, and 3.35 g (0.017 mol) of 2-(2-butyramido-ethyl)-thiophene are then added over the course of 15 minutes in such a way that the reaction temperature does not rise above 8°C. The ice bath is then removed and the reaction mixture is stirred for 30 minutes at 28°-30°C and then poured, whilst stirring, onto 100 g of ice under which there is a layer of 50 ml of methylene chloride. The methylene chloride phase is separated off and the aqueous phase is extracted with a further 50 ml of methylene chloride. The combined extracts are washed with 50 ml of concentrated sodium chloride solution, dried over sodium sulphate and evaporated at 40°C bath temperature with the aid of a rotary evaporator. The crude 5-(2-butyramido-ethyl)-2-thiophenesulphonyl chloride is obtained.

Provenance & Evidence