化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2012年
6期
1318-1320,1324
,共4页
徐东超%曲敏杰%姜殿平%李成斌%郭静%阮久勇
徐東超%麯敏傑%薑殿平%李成斌%郭靜%阮久勇
서동초%곡민걸%강전평%리성빈%곽정%원구용
(S)-乳酸乙酯%胺化反应%(S)-2-苄氧基丙醛%合成
(S)-乳痠乙酯%胺化反應%(S)-2-芐氧基丙醛%閤成
(S)-유산을지%알화반응%(S)-2-변양기병철%합성
ethyl(S)-lactate%amination reaction%(S)-2-benzyloxyl propanal%synthesis
(S)-2-苄氧基丙醛是有机合成及制药的重要中间体,本文以(S)-乳酸乙酯为原料,经四氢吡咯胺化、氯化苄醚化、红铝还原反应合成了(S)-2-苄氧基丙醛,考察了胺化的反应时间、反应温度和原料的摩尔比对反应收率的影响。结果表明:当胺化反应时间为75 h,最佳的反应温度为25℃,四氢吡咯与(S)-乳酸乙酯的摩尔比为1.4∶1时,胺化反应收率为94%,三步总收率为61.8%,采用GC-MS、IR、1H NMR表征确定了产物结构,研究结果为(S)-2-苄氧基丙醛的工业化生产奠定了基础。
(S)-2-芐氧基丙醛是有機閤成及製藥的重要中間體,本文以(S)-乳痠乙酯為原料,經四氫吡咯胺化、氯化芐醚化、紅鋁還原反應閤成瞭(S)-2-芐氧基丙醛,攷察瞭胺化的反應時間、反應溫度和原料的摩爾比對反應收率的影響。結果錶明:噹胺化反應時間為75 h,最佳的反應溫度為25℃,四氫吡咯與(S)-乳痠乙酯的摩爾比為1.4∶1時,胺化反應收率為94%,三步總收率為61.8%,採用GC-MS、IR、1H NMR錶徵確定瞭產物結構,研究結果為(S)-2-芐氧基丙醛的工業化生產奠定瞭基礎。
(S)-2-변양기병철시유궤합성급제약적중요중간체,본문이(S)-유산을지위원료,경사경필각알화、록화변미화、홍려환원반응합성료(S)-2-변양기병철,고찰료알화적반응시간、반응온도화원료적마이비대반응수솔적영향。결과표명:당알화반응시간위75 h,최가적반응온도위25℃,사경필각여(S)-유산을지적마이비위1.4∶1시,알화반응수솔위94%,삼보총수솔위61.8%,채용GC-MS、IR、1H NMR표정학정료산물결구,연구결과위(S)-2-변양기병철적공업화생산전정료기출。
Vanadium redox flow battery is a highly efficient storage energy installs.The electrolyte influence the battery capacity directly.(S)-2-benzyloxy propanal was synthesized by the amination of pyrrolidine,the etherification of benzyl chlorine and sodium bisaluminiumhydride with ethyl(S)-lactate as raw material.The reaction time,the reaction temperature and the mole ratio of raw material in the process of amination were investigated.The results showed that the yield of amination reaction was about 94% when amination reaction time was 72 h,the reaction temperature was 25 ℃ and the mole ratio of pyrrolidine to ethyl(S)-lactate was 1.4∶1.The overall yield was about 61.8%.The product structure was characterized and confirmed by GC-MS,IR and 1H NMR.The results provided important theoretical base for the industrial production of(S)-2-benzyloxy propanal.