Statistics shows that Sodium 2-bromoethanesulphonate is playing an increasingly important role. we look forward to future research findings about 4263-52-9.
Synthetic Route of 4263-52-9, These common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, 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.
A reactor was charged with 54.89 g (0.186 mol) methyloleate, 9.55 g (0.093 mol) diethylenetriamine and heated under an argon atmosphere with stirring to 160 C., whereupon methanol began to reflux, enough methanol was distilled off to bring to 180 C., stirring with argon sparging was continued for 2 days to yield pure 3-(2-((z)-hepatadec-8-en- 1 -y-1 -(2-oleamido ethyl)-4,5-dihydro- 1H-imidazoline as a viscous light straw colored fluid. ?3C NMR (ppm in CDC13, 100 MHz) oe=25.8, 36.6, 38.0, 46.6, 50.2, 52.2, 167.5, 173.4. A flask was charged with 4.000 g (6.514 mmol) 3-(2-((z)-hepatadec-8-en-1-yl)-1-(2-oleamido ethyl)-4,5-dihydro-1H-imidazoline, 1.648 g (7.810 mmol) sodium 2-bromoethylsulfonate, 20 ml anhydrous N-Methyl-2-pyrrolidone (NMP), heated under an argon atmosphere with stirring at 140 C. for 2 days. Evaporated the mixture in vacuo (90 C./0.8 mmHg), poured into 30 mL sodium chloride saturated deionized water, extracted with 20 mL aliquots of chloroform until the chloroform layer had only a faint color, combined the chloroform layer and dried over anhydrous magnesium sulfate, filtered through celite, vacuum distilled. A viscous dark amber fluid comprised of about 38 wt % of 2-(2-((Z)-heptadec-8-en-1-yl)-1-(2-oleamidoethyl)-4,5-dihydro-1H-imidazol-3-ium-3-yl)ethane-1-sulfonate (z-Im-1), 48 wt % Im and 15 wt % of NMP was obtained. The product was purified using flash chromatography with MeOH-water (9:1), and yield 80 mol % of z-IM-1. 13C NMR (ppm in CDCl3, 100 MHz) delta=170.8, 46.7, 47.4, 36.0, 46.3, 174.8, 25.7, 43.4, 45.7, 362, 25.6.
Statistics shows that Sodium 2-bromoethanesulphonate is playing an increasingly important role. we look forward to future research findings about 4263-52-9.
Reference:
Patent; GPCP IP Holdings LLC; Chen, Yu; Holtman, Kevin M.; Hammes, Brian S.; Boettcher, Jeffrey J.; (31 pag.)US2018/202109; (2018); A1;,
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