In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 703-12-8 as follows. Safety of 4-Bromo-N-methylbenzenesulfonamide
To a solution of 4-bromo-N-methylbenzenesulfonamide (2, 1.05 g, 4.20 mmol) and triisopropyl borate (1.45 mL, 6.30 mmol) in tetrahydrofuran (8.40 mL) was added n-Butyl Lithium (4.20 mL, 10.5 mmol) at -70 C. The mixture was slowly warmed to 0 C, then 10% HCl solution was added until pH 3-4. The resulting mixture was extracted with EtOAc. The organic layer was extracted with NaOH (2M) and the aqueous phase washed with diethyl ether. The aqueous phase was acidified to pH 3, extracted with EtOAc (impurities and unconsumed reactant were still present) was dried over Na2SO4, and evaporated under reduced pressure. The residue was triturated with diethyl ether to give [4- (methylsulfamoyl)phenyl]boronic acid (187 mg, 0,8700 mmol, 21% yield). (0781) Analytical data: (0782) 1H NMR (200 MHz, DMSO) delta 7.96 (d, J = 8.1 Hz, 2H), 7.72 (d, J = 8.0 Hz, 2H), 7.42 (q, J = 4.9 Hz, 1H), 2.39 (d, J = 5.0 Hz, 3H); (0783) 13C NMR (50 MHz, DMSO) delta 140.6, 134.8, 125.7, 28.8.
According to the analysis of related databases, 703-12-8, the application of this compound in the production field has become more and more popular.
Reference:
Patent; HEPAREGENIX GMBH; PRAEFKE, Bent; KLOeVEKORN, Philip; SELIG, Roland; ALBRECHT, Wolfgang; LAUFER, Stefan; (157 pag.)WO2019/149738; (2019); A1;,
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