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. 288148-34-5, name is 1-Methyl-1H-pyrazole-4-sulfonyl chloride, A new synthetic method of this compound is introduced below., Quality Control of 1-Methyl-1H-pyrazole-4-sulfonyl chloride
General procedure: A mixture of the appropriate (aryloxy)ethyl piperidine(0.38 mmol) in CH2Cl2 (3 mL), and TEA (1.14 mmol) was cooled down (ice bath), and arylsulfonyl chloride (0.46 mmol) was added at 0 C in one portion. The reaction mixture was stirred for 2-6 h under cooling. Then, the solvent was evaporated and the sulfonamides were purified using silica gel column with CH2Cl2/MeOH as an eluting system. Free bases were then converted into the hydrochloride salts by treatment of their solution in anhydrous ethanol with 1.25 M HCl in MeOH.; 9.2.6.8 1-Methyl-N-(1-{[2-(t-butyl-2-yl)phenoxy]ethyl}piperidin-4-yl)-N-methyl-1H-pyrazole-sulfonamide (17) Yellow oil, 80 mg following chromatographic purification over silica gel with CH2Cl2/MeOH (9:0.7); LC/MS purity 100%, tR = 4.81, C22H34N4O3S, MW 434.60, Monoisotopic Mass 434.24, [M+H]+ 435.5. 1H NMR (300 MHz, CDCl3) delta 1.37 (s, 9H), 1.50-1.58 (m, 2H), 1.70 (qd, J = 12.17, 3.89 Hz, 2H) 2.19 (td, J = 11.80, 2.23 Hz, 2H), 2.73 (s, 3H), 2.82 (t, J = 6.07 Hz, 2H), 2.97-3.04 (m, 2H), 3.76-3.88 (m, 1H), 3.93 (s, 3H), 4.06 (t, J = 6.06 Hz, 1H), 6.83 (dd, J = 8.21, 1.03 Hz, 1H), 6.87-6.91 (m, 1H), 7.15 (td, J = 7.71, 1.70 Hz, 1H), 7.27 (dd, J = 7.92, 1.44 Hz, 1H), 7.70 (s, 1H), 7.74 (s, 1H). 13C NMR (75 MHz, CDCl3) delta 28.58, 29.28, 29.68, 29.81, 34.81, 39.55, 53.48, 55.09, 57.13, 65.94, 112.03, 120.39, 122.24, 126.64, 126.97, 131.35, 138.10, 138.15, 157.49. Anal. calcd for C22H34N4O3S·2HCl: C: 52.06, H: 7.15, N: 11.04, S: 6.32; Found C: 51.95, H: 6.95, N: 10.82, S: 6.11. Mp for C22H34N4O3S·2HCl: 181.7-182.3 C.
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:
Article; Canale, Vittorio; Kurczab, Rafa?; Partyka, Anna; Sata?a, Grzegorz; S?oczy?ska, Karolina; Kos, Tomasz; Jastrz?bska-Wi?sek, Magdalena; Siwek, Agata; P?kala, Elzbieta; Bojarski, Andrzej J.; Weso?owska, Anna; Popik, Piotr; Zajdel, Pawe?; Bioorganic and Medicinal Chemistry; vol. 24; 2; (2016); p. 130 – 139;,
Pyrazole – Wikipedia,
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