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    • 2. 发明公开
    • 중수소로 치환된 올리고에틸렌티올분자 및 그 제조방법
    • 去离子水杨酸甘油三醇分子及其制备方法
    • KR1020120073128A
    • 2012-07-04
    • KR1020110140499
    • 2011-12-22
    • 건국대학교 산학협력단다이아텍코리아 주식회사
    • 여운석박형순최인성강현욱
    • C07C321/08C07C315/06G01N30/72
    • PURPOSE: An oligo(ethylene thiol) molecule substituted with deuterium and a manufacturing method thereof are provided to be used for mass analysis reference substance and to be applied in various fields. CONSTITUTION: A manufacturing method of an oligo(ethylene thiol) molecule substituted with deuterium comprises the following steps: a step of synthesizing 2-(2-(hex-5-enyloxy)ethoxy)ethanol or 2-(2-(undec-10-enyloxy)ethoxy)ethanol by reacting 6-bromohexene or 11-bromoundecene with NaOH solution and dithylene glycol mixed solution; a step of synthesizing 6-(2-(2-bromoethoxy)ethoxy)hex-1-ene or 11-(2-(2-bromo-ethoxy)ethoxy)undec-1-ene by reacting triphenyl phosphine and carbon tetrabromide with the product from the previous step; a step of synthesizing 2-(2-(2-(hex-5-enyloxy)ethoxy)ethoxy)ethanol-d4 or 2-(2-(2-(undec-10-enyloxy)ethoxy)ethoxy)ethanol-d4 by reacting NaH and ethylene glycol-D4 with the product from the previous step; a step of synthesizing S-6-(2-(2-(2-hydroxyethoxy)ethoxy)ethoxy)hexyl ethanethioate-d4 or S-11-(2-(2-(2-hydroxyethoxy)ethoxy)ethoxy)undecyl ethanethioate by reacting thioacetic acid and 2,2'-azobis(2-methylpropionamidine)dihydrochloride with the product from the previous step; and a step of synthesizing 2-(2-(2-(6-mercaptohexyloxy)ethoxy)ethoxy) ethanol-d4 or 2-(2-(2-(11-mercaptoundecyloxy)ethoxy)ethoxy)ethanol by reacting HCl with the product from the previous step.
    • 目的:用氘取代的低聚(乙烯硫醇)分子及其制造方法,用于质量分析参考物质,适用于各种领域。 构成:用氘取代的低聚(乙烯硫醇)分子的制造方法包括以下步骤:合成2-(2-(己-5-烯氧基)乙氧基)乙醇或2-(2-(十一碳-10-基) - 乙氧基)乙醇通过6-溴己烯或11-溴代癸酸与NaOH溶液和二亚乙基二醇混合溶液反应; 通过使三苯基膦和四溴化碳与四溴化碳反应合成6-(2-(2-(2-溴乙氧基)乙氧基)己-1-烯或11-(2-(2-溴 - 乙氧基)乙氧基)十一-1-烯) 产品从上一步; 乙氧基)乙氧基)乙氧基)乙醇-d4或2-(2-(2-(十一碳-10-烯氧基)乙氧基)乙氧基)乙醇-d4的步骤 将NaH和乙二醇-DD与前一步骤的产物反应; 合成S-6-(2-(2-(2-羟基乙氧基)乙氧基)乙氧基)乙基硫代乙酸酯-d4或S-11-(2-(2-(2-羟基乙氧基)乙氧基)乙氧基)十一烷基乙磺酸酯的步骤 将上述步骤中的产物与硫代乙酸和2,2'-偶氮双(2-甲基丙脒)二盐酸盐反应; 和通过HCl与产物反应合成2-(2-(2-(2-(6-巯基己氧基)乙氧基)乙氧基)乙醇-d4或2-(2-(2-(2-巯基十一烷氧基)乙氧基)乙氧基)乙醇)的步骤 从上一步。