Application of 3144-09-0, These common heterocyclic compound, 3144-09-0, name is Methylsulfonamide, 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.
CH2Cl2 (3.06 ml) was added to the 20 mL Scint vial containing DMAP (5.61 mg, 0.046 mmol), 2-chloro-1-methylpyridin-1-ium iodide (0.282 g, 1.102 mmol), benzoic acid 1a (0.1122 g, 0.919 mmol), methanesulfonamide 2a (0.175 g, 1.837 mmol) at room temperature. After stirring for 5 min, TEA (0.38 ml, 2.76 mmol) was slowly added to the reaction mixture. The reaction was stirred at room temperature for 1 hour. The reaction solvent was removed via vacuum and the crude was taken up in ethyl acetate, washed with 1N HCl. The ethyl acetate layer was separated, dried (Na2SO4), filtered and concentrated. The crude was purified by flash column eluted with ethyl acetate in hexane from 0 to 50% to 100% to give the desired product 3a as a white solid. (0.1409 g, 77%). 1H NMR (400 MHz, CHLOROFORM-d) delta 8.96 (br s, 1H), 7.95 – 7.82 (m, 2H), 7.68 – 7.61 (m, 1H), 7.56 – 7.49 (m, 2H), 3.46 (s, 3H); 13C NMR (126 MHz, CHLOROFORM-d) delta 165.5, 133.9, 131.0, 129.1, 127.9, 41.8; HRMS(ESI-) : observed: 198.0221; theory: 198.0217.
The synthetic route of 3144-09-0 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Chen, Ling; Luo, Guanglin; Tetrahedron Letters; vol. 60; 3; (2019); p. 268 – 271;,
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