Na-SG(Ⅰ)酯还原法合成2-(4-羟基苯)乙醇的研究  

APPLICATION OF Na-SG(Ⅰ) ESTER REDUCTIVE IN THE SYNTHESIS OF 2-(4-HYDROXYPHENYL)ETHANOL

作　　者：李运山[1] 邱玉华[1] 田梦云[1] 顾超力 

机构地区：[1]常州工程职业技术学院制药与生物工程技术系,江苏常州213164

出　　处：《精细石油化工》2015年第4期56-60,共5页Speciality Petrochemicals

基　　金：江苏省高等学校大学生实践创新训练计划资助项目(201313102011Y)

摘　　要：以4-羟基苯乙酸为原料,经阳离子交换树脂催化酯化反应和金属Na负载型硅胶Na-SG(Ⅰ)酯还原反应合成2-(4-羟基苯)乙醇,考察了工艺条件对各产物收率的影响。结果表明,较佳的酯化反应条件为:无水乙醇过量,催化剂用量占4-羟基苯乙酸用量的20%,回流反应2h,收率为95.8%;较佳的酯还原反应条件为:n(乙醇)∶n(钠)∶n(4-羟基苯乙酸乙酯)=8.0∶6.5∶1.0,溶剂无水四氢呋喃(THF)适量,0℃投料,室温反应30min,收率为98.6%。过程总收率为94.5%。分别用IR、HPLC和1 H NMR等对产物进行表征。2-（ 4-Hydroxyphenyl ） ethanol was prepared from 4-hydroxyphenylacetic acid through a route, esterification reaction on cation exchange resin and ester reductive reaction on Stage I sodium in silica gel. Effects of conditions on yields were investigated. Results showed that the optimal esteri-fication reaction conditions were as that ethanol overdosed, catalyst was 20% of the amount of 4- hydroxyphenylacetic acid and reflux reaction was for two hours, therefore, the yield of ethyl 4- hydroxyphenylacetate could be up to 95. 8%. The optimal ester reductive reaction conditions were as that n（ethyl alcohol）： n（sodium）： n（ethyl 4-hydroxyphenylacetate）=8.0： 6. 5：1.0, tetrahydrofu-ran （THF） in moderation was used as solvent, fed under 0℃ and reacted at room temperature for 30 minutes, therefore, the yield of 2-（4-hydroxyphenyl）ethanol could reach 98. 6%. The total yield was 94. 5% by this route. The target product was characterized by means of IR, HPLC, and 1H NMR.

关 键 词：Na-SG(Ⅰ) 还原 2-(4-羟基苯)乙醇 阳离子交换树脂 

分 类 号：TQ243.4[化学工程—有机化工]