d苯甘氨酸甲酯盐酸盐制备及纯化工艺研究化学工程与技术专业论文.docxVIP

万方数据 万方数据 河北科技大学硕士学位论文 II Abstract=========；暑=；昌昌============；==≈==；穹皇=========；号皇；=兰===昌==暑=======置==宣号=== Abstract =========；暑=；昌昌============；==≈==；穹皇=========；号皇；=兰===昌==暑=======置==宣号=== =： Abstract D。phenylglycine methyl ester hydrochloride，a type of white crystalline powder and important pharmaceutical intermediate，iS an essential active side chain for the production of cephalexin，cefaclor,and other IMactam antibiotics．In this paper,the synthesis and crystallization purification technique of D-phenylglycine methyl ester hydrochloride is systematically studied． The study on the synthesis of D—phenylglycine methyl ester hydrochloride．A preliminary synthetic route of D·phenylglycine methyl ester hydrochloride was designed， and sulfoxide chloride method was determined experimentally as a preferred synthetic route．In the experiment，the synthesis technique conditions such as the sequence of adding reagents，the ratio of reagents，the reaction temperature，the reflux time，and the adding rate of sulfoxide chloride were investigated and optimized．After the completion of the reaction，the vacuum azeotropic distillation and cooling crystallization with the temperature controlling should be done to the mother liquor．Finally through the post‘pmcessing，we can get．t11e crystal product of D—phenylglycine methyl ester hydrochloride．The purity of the product detected by using HPLC is more than 98．5％． with the yield more than 96％． The study on the thermodynamics of D-phenylglycine methyl ester hydrochloride crystallization．The solubility and supersolubility of D—phenylglycine methyl ester hydrochloride in six pure solvents(water，methanol，ethanol，acetone，ethyl acetate，and toluene)as well as in two kinds of binary mixed solvents with different compositions (methanol—ethyl acetate and methanol—toluene)were measured under the conditions of atmospheric pmssure and the temperature range of 283．1 5K-333．1 5K by using Laser Dynamics Method．Then the Apelblat equation，CNIBS／Redlich．