二苯基硅烷用于D-对羟基苯甘氨酸甲酯制备的新技术  

A New Technology for Preparing D-p-Hydroxyphenylglycine Methyl Ester with Diphenylsilane

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作  者:林韦康 江晓明 杨沫 相雪理 朱海 LIN Wei-kang;JIANG Xiao-ming;YANG Mo;XIANG Xue-li;ZHU Hai(Suqian Keylab Biochemical Co.,Ltd.,Suqian,Jiangsu 223800,China;Zhejiang Yuntao Biotechnology Co.,Ltd.,Shaoxing,Zhejiang 312369,China)

机构地区:[1]宿迁市科莱博生物化学有限公司,江苏宿迁223800 [2]浙江云涛生物技术股份有限公司,浙江绍兴312369

出  处:《浙江化工》2021年第4期21-26,共6页Zhejiang Chemical Industry

摘  要:为开发一种对设备腐蚀性小、生产成本低、产能大的D-对羟基苯甘氨酸甲酯生产新技术,尝试用二苯基硅烷作用于D-对羟基苯甘氨酸的甲酯化进程,效果较好。当V(无水甲醇):m(D-对羟基苯甘氨酸)=8.97 mL/g,反应温度为70℃,n(二苯基硅烷):n(D-对羟基苯甘氨酸)=1,反应时间为8 h时,实验结果最佳。目标产物摩尔收率为80.97%,外观为白色颗粒状晶状固体,含量(HPLC归一法)为99.16%,比旋光度为-150.23°,水分为0.21%,吸光度为0.013 AU,D-对羟基苯甘氨酸残留(HPLC归一法)为0.23%。In order to develop a new technology for the production of D-p-hydroxyphenylglycine methyl ester with less corrosive to equipment,low production cost and large production capacity,diphenylsilane is applied to the methyl esterification process of D-p-hydroxyphenylglycine,and the effect is good.When V(anhydrous methanolL):m(D-p-hydroxy phenylglycineg)=8.97 mL/g,reaction temperature was 70℃,n(diphenylsilane):n(D-p-hydroxy phenylglycine)=1,reaction time was 8 h,the best results were obtained.The molar yield of the target product was 80.97%,the appearance was white granular crystalline solid,the content(HPLC normalization)was 99.16%,the specific rotation was-150.23°,the moisture was 0.21%,the absorbance was 0.013 AU,and the D-p-hydroxyphenylglycine residue(HPLC normalization)was 0.23%.

关 键 词:D-对羟基苯甘氨酸甲酯 二苯基硅烷 酯化 

分 类 号:TQ245.24[化学工程—有机化工]

 

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