医药前沿
醫藥前沿
의약전연
Yiayao Qianyan
2015年
30期
360-362
,共3页
关东%陈新民%周爱新%李红钊
關東%陳新民%週愛新%李紅釗
관동%진신민%주애신%리홍쇠
手性去甲乌药碱%不对称合成
手性去甲烏藥堿%不對稱閤成
수성거갑오약감%불대칭합성
Chiral Higenamine%Asymmetric synthesis
以4-甲氧基苯乙酸及3,4-二甲氧基苯乙胺为起始原料,经过氯代、酰化缩合、环合、不对称还原、脱保护基等步骤,获得手性去甲乌药碱,本制备方法具有选择性高、简单、高效等优点,产物e e 。值达到95%以上,产物纯度高,且总收率可达30%,可实现规模制备。且其结构经元素分析,1HNMR,红外光谱和 MS 表征。
以4-甲氧基苯乙痠及3,4-二甲氧基苯乙胺為起始原料,經過氯代、酰化縮閤、環閤、不對稱還原、脫保護基等步驟,穫得手性去甲烏藥堿,本製備方法具有選擇性高、簡單、高效等優點,產物e e 。值達到95%以上,產物純度高,且總收率可達30%,可實現規模製備。且其結構經元素分析,1HNMR,紅外光譜和 MS 錶徵。
이4-갑양기분을산급3,4-이갑양기분을알위기시원료,경과록대、선화축합、배합、불대칭환원、탈보호기등보취,획득수성거갑오약감,본제비방법구유선택성고、간단、고효등우점,산물e e 。치체도95%이상,산물순도고,차총수솔가체30%,가실현규모제비。차기결구경원소분석,1HNMR,홍외광보화 MS 표정。
Chiral higenamine was prepared by chlorination, acylation, condensation, cyclization, asymmetric reduction and deprotection using 4 - methoxy phenyl acetic acid and 3,4 dimethyl phenyl ethylamine as the starting material. The preparation method which has the advantages of high selectivity, simple and efficient, the product ee. value reached more than 95%, the purity of the product is high and total yield up to 30%, achieve scale preparation. The structures were characterized by Element analysis, 1HNMR, IR and MS.