CAJ | 학술논문

在微波辐射条件下，以对羟基苯甲酸与乙醇为原料，SnCl4/C为异相催化剂，高效、绿色地合成对羟基苯甲酸乙酯。分别研究催化剂用量、醇酸摩尔比、反应时间、反应温度、微波辐射功率等对收率的影响，并采用傅里叶变换红外光谱（FT？IR）、核磁共振氢谱（1 H NMR）和质谱（MS）确定产物的结构。结果表明：合成对羟基苯甲酸乙酯最佳条件为n（对羟基苯甲酸）∶n（乙醇）＝1∶4，反应时间为25 min，催化剂的质量分数为10％，反应温度为120℃，微波辐射功率为640 W，产品收率为95％；SnCl4/C催化剂循环使用4次后，仍然显示出良好的催化活性，产率可达89％。
재미파복사조건하，이대간기분갑산여을순위원료，SnCl4/C위이상최화제，고효、록색지합성대간기분갑산을지。분별연구최화제용량、순산마이비、반응시간、반응온도、미파복사공솔등대수솔적영향，병채용부리협변환홍외광보（FT？IR）、핵자공진경보（1 H NMR）화질보（MS）학정산물적결구。결과표명：합성대간기분갑산을지최가조건위n（대간기분갑산）∶n（을순）＝1∶4，반응시간위25 min，최화제적질량분수위10％，반응온도위120℃，미파복사공솔위640 W，산품수솔위95％；SnCl4/C최화제순배사용4차후，잉연현시출량호적최화활성，산솔가체89％。
Ethyl p-hydroxylbenzoate was produced from p-hydroxy benzoic acid and ethanol as starting materials by u-sing SnCl4/C as efficient and green heterogeneous catalyst under microwave?assisted condition.The influences of the quantity of SnCl4/C,the ratio of acid and ethanol,and reaction time and temperature factors on the esterification yield are discussed.The structure of ethyl p-hydroxylbenzoate was characterized by Fourier-transform infrared spectroscopy (FT-IR),1H nuclear magnetic resonance spectroscopy (1H NMR)and mass spectroscopy (MS).The results showed that the optimal reactive conditions were as following:10% catalyst,the ration of acid and ethanol 1∶4,the radiation time 25 mi-nutes,the reaction temperature 120 ℃,the microwave power 640 W.Under the optimal reactive conditions,the yield of ethyl p-hydroxylbenzoate was up to 95%.Moreover,SnCl4/C catalyst can be recycled and reused at least 4 consecutive runs without a noticeable drop in the product yield (89%).