Research on new synthetic routes about N,N-Dimethyl-1H-pyrazole-1-sulfonamide

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, A new synthetic method of this compound is introduced below., COA of Formula: C5H9N3O2S

Step A: Preparation of3-Chloro-N,N-dimethyl- 1 H-pyrazole- 1-sulfonamideTo a solution of N-dimethylsulfamoylpyrazole (188.0 g,1.07 mol) in dry tetrahydrofuran (1500 mE) at 78 C. wasadded dropwise a solution of 2.5 M n-butyllithium (472 mE,1.18 mol) in hexane while maintaining the temperature below65 C. Upon completion of the addition the reaction mixturewas maintained at 78 C. for an additional 45 minutes, afterwhich time a solution of hexachloroethane (279 g, 1.18 mol)in tetrahydrofuran (120 mE) was added dropwise. The reac40 tion mixture was maintained for an hour at 78 C., warmedto 20 C. and then quenched with water (1 E). The reactionmixture was extracted with methylene chloride (4×500 mE);the organic extracts were dried over magnesium sulfate andconcentrated. The crude product was further purified by chro45 matography on silica gel using methylene chloride as eluentto afford the title product compound as a yellow oil (160 g).?HNMR(CDC13) oe 3.07 (d, 6H), 6.33 (s, 1H), 7.61 (s, 1H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; E I DU PONT DE NEMOURS AND COMPANY; Berger, Richard Alan; Annan, Isaac Billy; Lahm, George Philip; Flexner, John Lindsey; Selby, Thomas Paul; Stevenson, Thomas Martin; US9173400; (2015); B2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics