【作者】 王松林；

【导师】 赵林；

【作者基本信息】 天津大学 ， 化学工程， 2004， 硕士

【摘要】 DL—2—氨基—△2—噻唑啉—4—羧酸外消旋体（DL—ATC）是生物合成法制备L－半胱氨酸的前体，目前国内尚未实现工业化生产。后者又是广泛用于医药、化妆品和食品等领域的重要生物化学制品，市场需求量相当大。本论文阐述了由丙烯酸甲酯出发，经过氯化、脱氯化氢，加成，环合等步骤制备DL—2—氨基—△2—噻唑啉—4—羧酸（DL—ATC）工艺方法研究。以丙烯酸甲酯与其物质的量 0.03％～0.04％的苯醌阻聚剂混合，于 40～50℃通入氯气，制得 2，3－二氯丙酸甲酯（CPM）。由于采用在反应中通入空气，以增加溶解氧的工艺,不仅大大减少了阻聚剂的用量，并使收率达到 97％。同时还对后三步的反应条件进行了优化，简化了操作。2，3－二氯丙酸甲酯先与1.49 倍物质量的氢氧化钠在 25～30℃温度下反应 3h，然后再加入大约2倍物质的量的30％盐酸和等物质的量的硫脲于50～70℃反应3h。再与 1.5 倍物质的量的 25％氨水于 60～65℃反应，中和（pH＝6.4～6.7）闭环，过滤，洗涤得产品。收率近 75％，达到国际先进水平。此外，还研究了中试工艺路线，确定了中试工艺条件，进行了中试规模化的工艺设计，建成一套年产能力为 70 吨的生产装置，并用此装置生产出符合国外客户质量要求的合格产品，以及建立了用高效液相色谱法定量测定DL—ATC的方法。更多还原

【Abstract】 L-Cysteine is an important biochemical product which is widely used in themedical, cosmetic and food field. DL—2—Amino—△2—thiazoline－4－Carboxylicacid（DL—ATC）is a precursor of L-Cysteine. In the biosynthesis method. From methyl acrylate, DL—2—Amino—△2—thiazoline－4－Carboxylicacid （ DL — ATC ） was prepared through chlorination, dehydrochlorination,neutralization addition and cyclization reactions. Thus, A stream of chlorine isintroduced in a mixture of 1 portion methyl acrylate and 0.03%-0.04% portion ofp-Benzoquinone inhibitor, That the temperature of the mixture is maintained between40oC and 50oC.then metuyl acryeate is chlorinated to obtain 2,3-methyldichloropropianate. Polymerization of methyl acrylate during chlorination isdecreased greatly by using such inhibitor and the incerase quantity of the solubilisedoxygea by the introduce air into the reaction vessel.Yield of methyldichloropropianate can reach 97％。 The following three steps of reaction conditionwere optimized. Thus, 1mol of 2,3-methyl dichloropropianate reacted with about1.5mol of sodium hydrochloric in water at 25~30℃ for 3 hours. Then about 2mol30% hydrochloric acid and 1mol. of thiaurea were added and stirred at 50~70℃ for 3hours and finally 1.5mol 25% ammonium hydroxide was added. Neutralization,cyclization and filtering treatment were used to get the final product. In this way, notonly the procedures are simplified, but also the yield is increased from 72%. to about75%. Beside, the process of the middle-scale production was investigated .the processfor the production of DL—ATC was designed on the results of research work. Theequipment setting and running tests were accomplished and the high quality productswere obtained.The quantitative analytical method using HPLC is also established.更多还原