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. Quality Control of Sodium 2-bromoethanesulphonate
b) Compound lb; [0169] A mixture of compound la, (0.1 g, 0.45 mmole), sodium 2- bromoethanesulfonate (0.19 g, 2 equivalents) and 2,6-di-tert-butylpyridine (99 muL, 0.45 mmole) in [BMIM]BF4] (1 mL, Aldrich) was heated in an oil bath at 150C with vigorous stirring for 16 hours. The reaction was then cooled to room temperature and a small portion of the reaction mixture was withdrawn, diluted with methanol/water and analyzed by analytical HPLC using a Phenomenex, Ci8,4.6 x 250 mm column and a 30 minute gradient of 10? 70% MeCN/water (with 0.05% TFA) at a flow rate of 1.0 mL/minute and UV detection at 260nm and 220 nm. Product was observed eluting at Rt = 13.3 minutes (-40% conversion). The reaction mixture was prepared by diluting it with water (15 mL) and washing this solution with ethyl acetate (2 x 25 mL). The aqueous solution was then treated with 3 to 4 drops of ammonia and further extracted with ethyl acetate (2 x 25 mL). The aqueous solution was then concentrated to about 7 mL by rotary evaporation. The product was then purified by preparative HPLC using an YMC, Ci8, 30 x 250 mm column and the same gradient as described above at a flow rate of 20 mL/minute. HPLC fractions containing product were combined and concentrated under reduced pressure. Yield = 30 mg (20%, white solid); MALDI-TOF MS 330.6 observed.
The synthetic route of Sodium 2-bromoethanesulphonate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SIEMENS HEALTHCARE DIAGNOSTICS INC.; NATRAJAN, Anand; SHARPE, David; WEN, David; JIANG, Qingping; WO2011/146595; (2011); A2;,
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bromide – Wiktionary