Chlorosulfonic acid → HCID 178433697, compound

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Reaction Steps

133 ml (0.002 mol) of chlorosulphonic acid is added, with stirring, to a solution of 0.72 ml (0.0042 mol) of N,N-diisopropylethylamine in 12 ml of a 1/1 chloroform/dimethylformamide mixture, cooled in ice. After a waiting time of 30 minutes, 0. 168 g (0.001 mol) of 2-methyl-4-amino-6-dimethylaminopyrimidine 3-oxide prepared according to Example 2 is added and the mixture is kept at between 5° and 10° C. for 7 hours under nitrogen. The solvent is evaporated. The residue, taken up in a little water, allows a white product to crystallise, which is filtered off. After recrystallisation from a DMF/water mixture, 0.11 g of pure inner salt, which decomposes at 226° C., is obtained. The yield is 44.3%. Elementary analysis for C7H12N4O4S; molecular weight=248.

Provenance & Evidence