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作 者:郭庆君 Guo Qingjun(School of Chemistry,Chemical Engineering and Materials,Jining University,Qufu 273155,China)
机构地区:[1]济宁学院化学化工与材料学院,山东曲阜273155
出 处:《山东化工》2022年第13期36-39,43,共5页Shandong Chemical Industry
摘 要:在常温下,水溶液中,使用水溶性金属配合物做催化剂,添加相转移剂PPNCl,使溶进水中的苯甲酰乙腈被甲酸还原成氰甲基苄醇;优选了反应的最佳条件为n_(苯甲酰乙腈)∶n_(甲酸)∶n_(催化剂)∶n_(相转移剂)=1∶6∶0.005∶0.02;通过高效液相色谱法(HPLC)测试,获得产物的对映体过量值e.e.,在最佳反应条件下,产物对映体过量值e.e.是87.3%,转化率为96.5%;产物经^(1)H NMR和^(13)C NMR确证结构,分子构型经旋光度测试并与文献报道比对确定为S型。Using water-soluble metal complex as catalyst and phase transfer agent PPNCl,benzoyl acetonitrile was reduced to cyanomethyl benzyl alcohol by formic acid in aqueous solution at room temperature.The optimum reaction conditions were n(benzoyl acetonitrile)∶n(formic acid)∶n(catalyst)∶n(phase transfer agent)=1∶6∶0.005∶0.02.The enantiomer oversize value of the product was obtained by high performance liquid chromatography(HPLC).Under the optimal reaction conditions,the enantiomer oversize value of the product was e.e.87.3%,conversion rate is 96.5%.The structure of the product was confirmed by^(1)H NMR and^(13)C NMR and its molecular configuration was determined as S-type by spectrophotometry test and comparison with literature reports.
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