Reference of 133228-21-4, The chemical industry reduces the impact on the environment during synthesis 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, I believe this compound will play a more active role in future production and life.
To a solution of N,N-dimethylsulfamoylpyrazole (44.0 g, 0.251 mol) in dry tetrahydrofuran (500 ml) at -78C was added dropwise a solution of n-butyllithium (2.5 M in hexane, 105.5 ml, 0.264 mol) while maintaining the temperature below -60C. A thick solid formed during the addition. Upon completion of the addition the reaction mixture was maintained for an additional 15 minutes, after which time a solution of 1,2-dibromotetrachloroethane (90 g, 0.276 mol) in tetrahydrofuran (150 ml) was added dropwise while maintaining the temperature below -70C. The reaction mixture turned a clear orange; stirring was continued for an additional 15 minutes. The -78C bath was removed and the reaction was quenched with water (600 ml). The reaction mixture was extracted with methylene chloride (4x), and the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using methylene chloride-hexane (50 : 50) as eluent to afford 57.04 g of the title product as clear colorless oil. 1H NMR (CDCl3): delta 3.07 (d, 6H), 6.44 (m, 1H), 7.62 (m, 1H).
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