CAJ | 학술논문

以硫代乙酸、甲基丙烯酸为原料,经过缩合、水解-酯化得到3-苯甲酰巯基-2-甲基丙酸的消旋体,经化学拆分得到（S）-3-苯甲酰巯基-2-甲基丙酸。综合考察了缩合、水解-酯化、拆分过程中影响反应的因素,结果表明：硫代乙酸与甲基丙烯酸摩尔比为1.4︰1,反应时间为2 h、反应温度为93℃条件下,可以得到收率为95.6%的3-乙酰巯基-2-甲基丙酸（缩合物A）;控制釜温不超过20℃,将缩合物A加入11.8%的氢氧化钠水溶液中进行水解,水解完成后将下层钠盐投回釜内,然后在低温下滴加苯甲酰氯,反应进行2 h后将釜液调至酸性,产品逐渐析出,计算得水解-酯化总收率为96.7%;利用拆分剂D-（＋）-N-苄基-α-苯乙胺对产品拆分,拆分收率为36.0%,综合以上三步总收率可达33.3%。其结构经核磁、质谱、红外分析确认且由X射线衍射分析结晶度非常高。
이류대을산、갑기병희산위원료,경과축합、수해-지화득도3-분갑선구기-2-갑기병산적소선체,경화학탁분득도（S）-3-분갑선구기-2-갑기병산。종합고찰료축합、수해-지화、탁분과정중영향반응적인소,결과표명：류대을산여갑기병희산마이비위1.4︰1,반응시간위2 h、반응온도위93℃조건하,가이득도수솔위95.6%적3-을선구기-2-갑기병산（축합물A）;공제부온불초과20℃,장축합물A가입11.8%적경양화납수용액중진행수해,수해완성후장하층납염투회부내,연후재저온하적가분갑선록,반응진행2 h후장부액조지산성,산품축점석출,계산득수해-지화총수솔위96.7%;이용탁분제D-（＋）-N-변기-α-분을알대산품탁분,탁분수솔위36.0%,종합이상삼보총수솔가체33.3%。기결구경핵자、질보、홍외분석학인차유X사선연사분석결정도비상고。
3-benzoylthio-2-methylpropionic acid racemate was synthesized by condensation and hydrolysis-esterification reaction of thioacetic acid with methacrylic acid, then （S）-3-benzoylthio- 2-methylpropionic acid was obtained by chemical resolution. The influencing factors in each step were taken into account. The results showed that 3-acetyl-mercapto-2-methyl-propionic acid （ condensate A ） was obtained with the yield of 95.6% when the molar ratio of thioacetic acid to methacrylic acid was 1.4 ： 1, reaction time was 2h and reaction temperature was 93 ~C. Condensate A was added into 11.8% sodium hydroxide aqueous solution to make it hydrolysis with kettle temperature below 20 ~C, then sodium salt was put into the kettle, and the same mole benzoyl chloride was dropped as condensate A into the kettle under low temperature. Two hours later, the product was obtained by acidifying the reaction mixture with hydrochloric acid, the yield of product in hydrolysis-esterification reaction was 96.7%. D-（＋）-N-benzyl-a-phenylethylamine was used as the resolving agent to split the product, the yield in this step was 36%. Taking all the procedures above into consideration, the yield of final product was 33.3%. The product was characterized with MS, ~H NMR and FT-IR analysis, and proved to be with high crystallinity by X ray diffraction.