Water → HCID 23312051, compound

Participants

Reaction Steps

3.88 g (0.0069 mol) of 5-chloro-6-(4-chlorophenylsulphonyl)-1,3-benzodioxole-2-carboxylic acid ethyl ester are dissolved in 20 ml of dimethylformamide and are added to 0.71 g (0.012 mol) of guanidine at room temperature. The mixture is stirred for 2 hours at room temperature, then poured out onto 200 ml of water. After stirring for 1/2 hour, a crystalline suspension has formed. This is filtered, washed with water, and the crude product is dried in a vacuum drying chamber at 30°-40°. The crude product is then digested with 25 ml of ethyl acetate, partial dissolution and recrystallisation occurring. The whole is cooled for 1/2 hour in an ice-bath, filtered and dried, yielding, in the form of beige crystals, 5-chloro-6-(4-chlorophenylsulphonyl)-1,3-benzodioxole-2-carboxylic acid guanidide having a melting point of from 215° (decomposition).

Provenance & Evidence