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研究了以羧酸酐和羟基芳磺酸盐为主要原料,丙酮为溶剂、无水碳酸钠为缚酸剂的烷酰氧基芳磺酸盐的清洁合成工艺,制备了4-壬酰氧基苯磺酸钠(NOBS)、壬酰氧基尼文酸钠、4-甲基丙烯酰氧基苯磺酸钠、甲基丙烯酰氧基尼文酸钠等4个化合物.考察了合成反应的影响因素.结果表明,以对羟基苯磺酸钠和壬酸酐为原料合成4-壬酰氧基苯磺酸钠(NOBS)的收率和含量均最高,优化条件为n(对羟基苯磺酸钠)∶n(壬酰酐)∶n(无水碳酸钠)=1∶1.3∶1.5,丙酮为溶剂,反应温度0℃～5℃,反应时间3 h,收率为90.7%,w(NOBS)=95.5%,通过红外光谱和核磁共振验证了目标产物.
The clean synthesis of alkanoyloxyarylsulfonates with carboxylic anhydride and hydroxyaromatic sulfonate as main raw materials, acetone as solvent and anhydrous sodium carbonate as acid-binding agent was studied. 4-Nonanoyloxybenzene (NOBS), sodium nonanoyloxy nalinate, sodium 4-methacryloyloxybenzenesulfonate and sodium methacryloyloxy nalinate, etc. The factors affecting the synthesis were investigated. The results showed that the yield and content of sodium 4 - nonanoyloxybenzenesulfonate (NOBS) synthesized from sodium p - hydroxybenzenesulfonate and nonanoic anhydride were the best. The optimum conditions were n (sodium p - hydroxybenzenesulfonate): n (nonanoyl anhydride): n (anhydrous sodium carbonate) = 1: 1.3: 1.5, acetone as solvent, reaction temperature 0 ℃ ~ 5 ℃, reaction time 3 h, yield 90.7% %, Confirmed by infrared spectroscopy and nuclear magnetic resonance of the target product.