公开(公告)号：US08519191B2

公开(公告)日：2013-08-27

申请号：US13142716

申请日：2010-03-12

申请人： Zhongfa Zhang ,  Xueyang Guo ,  Hui Huang

发明人： Zhongfa Zhang ,  Xueyang Guo ,  Hui Huang

IPC分类号： C07C213/04 ,  C07C213/02

CPC分类号： C07C213/02 ,  C07C213/10 ,  C07C215/10

摘要： A synthesis method of 3-methylamino-1,2-propanediol is disclosed in the invention, and it includes the following steps: (a) adding glycerin chlorohydrin, aqueous monomethylamine solution and an amination catalyst, namely NaOH solution and NaHCO3, into a reactor, mixing the material sufficiently, and allowing amination reaction to proceed in two temperature stages; (b) removing monomethylamine and water from the amination solution after the amination reaction is completed, filtering out the solid resultant, and feeding the filtrate into a still; (c) distilling under reduced pressure to obtain 3-methylamino-1,2-propanediol, wherein the vacuum for distillation under reduced pressure is equal to or greater than 0.099 MPa and the temperature is 130-160° C.

摘要翻译： 本发明公开了3-甲基氨基-1,2-丙二醇的合成方法，其包括以下步骤：（a）将甘油氯醇，一甲胺水溶液和胺化催化剂即NaOH溶液和NaHCO 3加入到反应器 ，充分混合该材料，并允许胺化反应在两个温度阶段进行; （b）在胺化反应完成后从胺化溶液中除去一甲胺和水，过滤固体产物，并将滤液送入静止液中; （c）在减压下蒸馏得到3-甲基氨基-1,2-丙二醇，其中减压蒸馏的真空度等于或大于0.099MPa，温度为130-160℃。

公开(公告)号：US20120277471A1

公开(公告)日：2012-11-01

申请号：US13142716

申请日：2010-03-12

申请人： Zhongfa Zhang ,  Xueyang Guo ,  Hui Huang

发明人： Zhongfa Zhang ,  Xueyang Guo ,  Hui Huang

IPC分类号： C07C213/10

CPC分类号： C07C213/02 ,  C07C213/10 ,  C07C215/10

摘要： A synthesis method of 3-methylamino-1,2-propanediol is disclosed in the invention, and it includes the following steps: (1) adding glycerin chlorohydrin, aqueous monomethylamine solution and an amination catalyst, namely NaOH solution and NaHCO3, into a reactor, mixing the material sufficiently, and allowing amination reaction to proceed in two temperature stages; (2) removing monomethylamine and water from the amination solution after the amination reaction is completed, filtering out the solid resultant, and feeding the filtrate into a still; (3) distilling under reduced pressure to obtain 3-methylamino-1,2-propanediol, wherein the vacuum for distillation under reduced pressure is equal to or greater than 0.099 MPa and the temperature is 130-160° C. The product synthesized according to the invention, a liquid appearing colorless and transparent, has increased purity of over 99.5% (GC) and decreased impurities. Therefore, when this product is used for synthesis of iopromide as a hypo-osmolar nonionic contrast medium, it exactly meets the quality demand.

摘要翻译： 本发明公开了3-甲基氨基-1,2-丙二醇的合成方法，其包括以下步骤：（1）将甘油氯醇，一甲胺水溶液和胺化催化剂即NaOH溶液和NaHCO 3加入到反应器 ，充分混合该材料，并允许胺化反应在两个温度阶段进行; （2）胺化反应完成后，从胺化溶液中除去一甲胺和水，滤出固体产物，并将滤液送入静止液中; （3）减压蒸馏得到3-甲基氨基-1,2-丙二醇，其中减压蒸馏的真空度等于或大于0.099MPa，温度为130-160℃。根据 本发明的液体无色透明，纯度提高超过99.5％（GC），杂质降低。 因此，当该产品用于合成碘普胺作为低渗透非离子型造影剂时，其完全符合质量要求。