安徽化工
安徽化工
안휘화공
ANHUI CHEMICAL INDUSTRY
2014年
2期
14-16,26
,共4页
云迪%刘敬茹%吴亚先%何黎琴
雲迪%劉敬茹%吳亞先%何黎琴
운적%류경여%오아선%하려금
大黄酸%甘氨酸甲酯盐酸盐%合成
大黃痠%甘氨痠甲酯鹽痠鹽%閤成
대황산%감안산갑지염산염%합성
Rhein%methylglycinate%synthesis
目的：合成大黄酰甘氨酰甘氨酸并对其合成工艺进行优化。方法：以大黄酸为原料，制成酰氯后与甘氨酸甲酯反应得大黄酰甘氨酸甲酯，酯基水解得大黄酰甘氨酸，再与甘氨酸甲酯在DMAP/EDCI作用下生成大黄酰甘氨酰甘氨酸甲酯，最后水解得大黄酰甘氨酰甘氨酸。结果与结论：设计并合成了大黄酰甘氨酰甘氨酸，目标化合物经IR、1H-NMR、MS等方法验证，同时优化了合成工艺，总收率达41.9%（以大黄酸计）。
目的：閤成大黃酰甘氨酰甘氨痠併對其閤成工藝進行優化。方法：以大黃痠為原料，製成酰氯後與甘氨痠甲酯反應得大黃酰甘氨痠甲酯，酯基水解得大黃酰甘氨痠，再與甘氨痠甲酯在DMAP/EDCI作用下生成大黃酰甘氨酰甘氨痠甲酯，最後水解得大黃酰甘氨酰甘氨痠。結果與結論：設計併閤成瞭大黃酰甘氨酰甘氨痠，目標化閤物經IR、1H-NMR、MS等方法驗證，同時優化瞭閤成工藝，總收率達41.9%（以大黃痠計）。
목적：합성대황선감안선감안산병대기합성공예진행우화。방법：이대황산위원료，제성선록후여감안산갑지반응득대황선감안산갑지，지기수해득대황선감안산，재여감안산갑지재DMAP/EDCI작용하생성대황선감안선감안산갑지，최후수해득대황선감안선감안산。결과여결론：설계병합성료대황선감안선감안산，목표화합물경IR、1H-NMR、MS등방법험증，동시우화료합성공예，총수솔체41.9%（이대황산계）。
Objective:To synthesize Rheinoyl glycylglycine and optimize the technical process. Methods:Rhein was reacted with thionyl chloride to get rheinoyl chloride, which was condensed glycin methylate to yield rheinoyl glycin methlate. The rheinoyl glycin methlate was hydrolyzed to give rheinoyl glycine. The target compound was gained by coupling with the glycin methylate to rheinoyl glycine and subsequent demethylation. Results and Conclusion:The target compound was obtained. Its chemical structure was confirmed by MS, IR, and 1H-NMR spectra. The yield of rheinoyl glycylglycine was 41.9%.
