1-氨基-3-(二甲氨基)丙-2-醇盐酸盐的合成  

Synthesis of 1-amino-3-(dimethylamino)propan-2-ol hydrochloride

作　　者：汪小兵 尹先清[1] 李强[2] 李立威[2] 

机构地区：[1]长江大学化学与环境工程学院,湖北荆州434023 [2]荆楚理工学院湖北省荆门医药工业技术研究院,湖北荆门448000

出　　处：《化学工程师》2018年第1期11-14,共4页Chemical Engineer

基　　金：湖北省高等学校优秀中青年科技创新团队计划项目(T200911)

摘　　要：以邻苯二甲酰亚胺钾盐为起始原料,与环氧氯丙烷缩合制得N-(2,3-环氧丙基)邻苯二甲酰胺,再和二甲胺在密闭环境中加热发生亲核加成开环反应,得到N-[3-(二甲氨基)-2-羟丙基]邻苯二甲酰胺,最后再用水合肼脱去邻苯二甲酰基得到1-氨基-3-(二甲氨基)丙-2-醇,1-氨基-3-(二甲氨基)丙-2-醇成盐得目标产物。经过正交优化,关键步骤开环反应在温度为75℃、反应时间为6.0h、物料比为1∶2.5时收率可达75%。所有化合物经MS、~1H NMR、^(13)C NMR等确证结构。该合成方法简单易行,反应条件温和,总收率可达55%,能有效合成出氨基不对称取代的1,3-二氨基-2-丙醇这类重要的中间体。2-（oxiran-2-ylmethyl）isoindoline-1,3-dione was prepared by condensation reaction,with epichloroh-ydrin and phthalimide potassium salt which as its -starting material.2-（3-（di-methylamino）-2-hydrox- ypropyl） isoindoline-1,3-dione was synthesized by 2-（oxiran-2-ylme-thyl）isoindoline-1,3-dione and dimethy- lamine which react in a high temperature sealed environment to open the epoxy ring and nucleophilic addition.At last,2-（3-（dimethylamino）-2--hydroxypropyl）isoindolinel,3-dione take off the protective group to obtain the products.After orthogonal test, when the reaction temperature was 75℃, reaction time was 6.0h, the feed ratio was 1： 2.5,ring opening reaction yield was 75%,All the compounds were characterized by MS, 1H NMR and 13C NMR.The synthesis process is simple and reaction conditions are mild,the total yield was 55% ,therefore, an import-ant in- termediate such as 1,3-diamin opropan-2-ol,which is asymmetrically substituted by amino groups can be effi- ciently synthesized.

关 键 词：邻苯二甲酰亚胺钾盐 环氧氯丙烷 二甲氨基 合成 

分 类 号：O623.42[理学—有机化学]