武汉轻工大学学报
武漢輕工大學學報
무한경공대학학보
Journal of Wuhan Polytechnic University
2015年
3期
52-56
,共5页
陈芬%覃宇%李建芬%王强胜%熊志翀
陳芬%覃宇%李建芬%王彊勝%熊誌翀
진분%담우%리건분%왕강성%웅지충
吲哚%医药中间体%合成%表征%工艺
吲哚%醫藥中間體%閤成%錶徵%工藝
신타%의약중간체%합성%표정%공예
indole%pharmaceutical intermediates%synthesis%characterization%research on process
探究2-吲哚乙酸乙酯新的合成方法和合成工艺。以2-硝基苯乙酸和丙二酸二乙酯为原料,通过亲核加成和还原环化反应,合成2-吲哚乙酸乙酯,关键合成步骤以不同的物料比、温度和反应时间进行反应,测得最终反应的转化率和产率,得到新的合成路线和最佳合成工艺。合成的最终产物为浅棕色固体,熔点为28—31℃,利用IR、1 HNMR和MS等分析手段对中间体和终产物的结构进行了表征和分析,确认最终产物即为目标产物2-吲哚乙酸乙酯。新的合成方法反应条件温和,中间体产物无须分离,关键步骤最佳合成工艺为:物料配比n(2-硝基苯乙酸):n(丙二酸单乙酯钾盐)为1∶2,反应温度5℃,反应时间为20 h,此时产品收率达87.5%,色谱检测纯度≥98%。
探究2-吲哚乙痠乙酯新的閤成方法和閤成工藝。以2-硝基苯乙痠和丙二痠二乙酯為原料,通過親覈加成和還原環化反應,閤成2-吲哚乙痠乙酯,關鍵閤成步驟以不同的物料比、溫度和反應時間進行反應,測得最終反應的轉化率和產率,得到新的閤成路線和最佳閤成工藝。閤成的最終產物為淺棕色固體,鎔點為28—31℃,利用IR、1 HNMR和MS等分析手段對中間體和終產物的結構進行瞭錶徵和分析,確認最終產物即為目標產物2-吲哚乙痠乙酯。新的閤成方法反應條件溫和,中間體產物無鬚分離,關鍵步驟最佳閤成工藝為:物料配比n(2-硝基苯乙痠):n(丙二痠單乙酯鉀鹽)為1∶2,反應溫度5℃,反應時間為20 h,此時產品收率達87.5%,色譜檢測純度≥98%。
탐구2-신타을산을지신적합성방법화합성공예。이2-초기분을산화병이산이을지위원료,통과친핵가성화환원배화반응,합성2-신타을산을지,관건합성보취이불동적물료비、온도화반응시간진행반응,측득최종반응적전화솔화산솔,득도신적합성로선화최가합성공예。합성적최종산물위천종색고체,용점위28—31℃,이용IR、1 HNMR화MS등분석수단대중간체화종산물적결구진행료표정화분석,학인최종산물즉위목표산물2-신타을산을지。신적합성방법반응조건온화,중간체산물무수분리,관건보취최가합성공예위:물료배비n(2-초기분을산):n(병이산단을지갑염)위1∶2,반응온도5℃,반응시간위20 h,차시산품수솔체87.5%,색보검측순도≥98%。
To explore the new method for synthesizing 2-indole acetic acid ethyl ester , and research the synthesis process.2-indoleacetic acid ethyl ester is synthesized by the nucleophilic addition and the reductive cyclisation re -actions using 2-nitrophenyl acetic acid and diethyl malonate as raw materials ,a new synthetic route was obtain and the best synthesis processin were optimized , through the determination of the last reaction conversion rate and yield , with different raw material ratio , reaction temperature and reaction time reaction time and temperature of reaction in the key step of synthesis .The final product synthesis is light brown solid , the melting point of about 28-31℃, by u-sing IR and 1 HNMR, MS and other analytical methods , the structure of the intermediates and the end products were characterized and analyzed , confirming the final product is the target product 2-indoleacetic acid ethyl ester .The new synthesis method has the advantages of mild reaction conditions , intermediate products do not need to be sepa-rated,and the synthesis process of the key steps is best material ratio n (2-nitrophenyl acetic acid ):n ( ethyl mal-onate potassium salt) was 1:2, reaction temperature was 5 C, reaction time was 20h, at this condition ,the yield was 87 .5%, the chromatographic purity was more than 98%.