CAJ | 학술논문

在水相中，相转移催化剂催化条件下合成1‐甲基‐5‐巯基‐1H‐四氮唑，并对其工艺条件进行研究．采用IR与1 HNM R对产物结构进行了表征．结果表明催化剂的最优制备条件为：催化剂为环糊精、蒸馏水加入量为30 m L、催化剂加入量为1％（占叠氮钠的摩尔百分数）．在此催化条件下优化工艺条件为：异硫氰酸甲酯与叠氮钠的摩尔比为1．4∶1．0；滴加完异硫氰酸甲酯后的反应时间为2 h；反应温度为75℃．产物收率为76．93％．
재수상중，상전이최화제최화조건하합성1‐갑기‐5‐구기‐1H‐사담서，병대기공예조건진행연구．채용IR여1 HNM R대산물결구진행료표정．결과표명최화제적최우제비조건위：최화제위배호정、증류수가입량위30 m L、최화제가입량위1％（점첩담납적마이백분수）．재차최화조건하우화공예조건위：이류청산갑지여첩담납적마이비위1．4∶1．0；적가완이류청산갑지후적반응시간위2 h；반응온도위75℃．산물수솔위76．93％．
In the presence of phase‐transfer catalyst ,5‐mercapto‐1‐methyltetrazole was syn‐thesized in aqueous phase .The structure was characterized by means of IR and 1 H NMR .The optimum condition of phase transfer catalyst were ascertained as follows :the phase transfer catalyst was cyclodextrin ,the quality of deionized water was 30 mL ,and the quality ratio of phase transfer catalyst and sodium azide was 1∶100(mol/mol) .Using cyclodextrin as phase transfer catalyst ,the optimum preparation procedure was :reaction temperature was 70 ℃ , the quality ratio of methyl isothiocyanate and sodium azide was 1 .4∶1 .0 (mol/mol) ,reac‐tion time was 2 h ,and the yield of 5‐mercapto‐1‐methyltetrazole was 79 .63% .