微波辐射技术合成3-氯-2-羟基丙磺酸钠

在微波辐射下,以环氧氯丙烷和亚硫酸氢钠为原料、去离子水为溶剂、四丁基溴化铵为相转移催化剂合成了3-氯-2-羟基丙磺酸钠;通过熔点测定和红外光谱分析对产物结构进行了表征;考察了原料配比、催化剂用量、反应温度、微波辐射功率、环氧氯丙烷滴加时间等因素对产物收率的影响。实验结果表明,微波辐射可明显促进3-氯-2-羟基丙磺酸钠的合成,在 n(亚硫酸氢钠):n(环氧氯丙烷):n(四丁基溴化铵)=1∶1.4∶0.0078、反应温度85℃、环氧氯丙烷滴加时间20 min、后续回流7 min、微波辐射功率500 W、微波辐射时间27 min 时,3-氯-2-羟基丙磺酸钠的收率可达85.8%。该方法具有操作简便、反应时间短、产物收率高等特点。

Synthesis of Sodium 3-Chloro-2-Hydroxy Propanesulfonate Under Microwave Irradiation

Sodium 3-chloro-2-hydroxy propanesulfonate was synthesized from epichlorohydrin and sodium bisulfite under microwave radiation,using deionized water as solvent and tetrabutyl ammonium bromide as phase transfer catalyst.Structures of products were identified by micro-melting point measuring instrument and IR spectrometer.Experimental results show that microwave radiation tremendously enhanced the yield of sodium 3-chloro-2-hydroxy propanesulfonate.Effects of reactant ratio,dropping time of epichlorohydrin,catalyst dosage,microwave irradiaton power,and irradiation time on reaction were studied.Under optimal reaction conditions:n(sodium bisulfite): n(epichlorohydrin):n(tetrabutyl ammonium bromide)=1:1.4:0.0078,reaction temperature 85℃,dropping time of epichlorohydrin 20 min,reflux time 7 min,microwave irradiation power 500 W and irradiation time 27 min,yield of sodium 3-chloro-2-hydroxy propanesulfonate is 85.8%.This method features short reaction time,high yield and simple operation.