These common heterocyclic compound, 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. SDS of cas: 133228-21-4
17(1) 1-(Dimethylsulfamoyl)-5-(2-chloro-6-methylphenylthio)pyrazole 32.3 ml of a 1.59M solution of butyllithium in hexane were added, at -78 C. and under an atmosphere of nitrogen, to a solution of 8.18 g of 1-(dimethylsulfamoyl)pyrazole [prepared as described in Example 1(1)] in 250 ml of dry tetrahydrofuran, and the resulting mixture was allowed to stand at the same temperature for 40 minutes. At the end of this time, a solution of 14.73 g of 2-chloro-6-methylphenyl disulfide in 100 ml of tetrahydrofuran was added to the mixture, which was then stirred at the same temperature for 1 hour. The reaction mixture was then mixed with an aqueous solution of ammonium chloride and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate, after which it was concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, eluted with a 10:1 by volume mixture of hexane and ethyl acetate, to give 13.70 g (yield 88%) of the title compound as an oil. Nuclear Magnetic Resonance Spectrum (CDCl3, 200 MHz), delta ppm: 7.48 (1H, doublet, J=1.6 Hz); 7.45-7.27 (3H, multiplet); 5.32 (1H, doublet, J=1.6 Hz); 3.05 (6H, singlet); 2.53 (3H, singlet).
The synthetic route of N,N-Dimethyl-1H-pyrazole-1-sulfonamide has been constantly updated, and we look forward to future research findings.