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以苯甲醛和氯乙酸乙酯为原料,经Darzens缩合反应合成了反式-3-苯基缩水甘油酸乙酯,然后在25℃以氨水开环得赤型-3-苯基异丝氨酰胺。赤型-3-苯基异丝氨酰胺在对甲苯磺酸存在下与甲醇回流24h,再以苯甲酰氯酰化得赤型-N-苯甲酰基-3-苯基异丝氨酸甲酯。赤型-N-苯甲酰基-3-苯基异丝氨酸甲酯以二氯亚砜翻转C-2位构型生成苏型-N-苯甲酰基-3-苯基异丝氨酸甲酯。苏型-N-苯甲酰基-3-苯基异丝氨酸甲酯在0℃水解即得紫杉醇C-13侧链苏型-N-苯甲酰基-3-苯基异丝氨酸。 相似文献
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(2R,3S) N 苯甲酰基 3 苯基异丝氨酸,是抗癌新药紫杉醇的侧链。利用苯甲醛和氯乙酸乙酯为原料,在甲醇钠作用下,0℃经Darzen反应24h,蒸去甲醇,乙醚萃取,减压蒸馏得到反式 3 苯基缩水甘油酸乙酯(4),4的甲醇溶液与NH3在100℃中压下氨解,在V(CH2Cl2)/V(CH3OH)=1∶1溶剂中结晶得赤式 3 苯基异丝氨酰胺(5),5在100℃用Ba(OH)2水解8h,得到赤式 3 苯基异丝氨酸(6),6与苯甲酰氯于0℃下在w(NaHCO3)=10%的溶液中发生酰化反应,V(THF)/V(CH2Cl2)=4∶1溶剂萃取,粗产物在V(石油醚)/V(丙酮)=40∶1溶剂中结晶,得到赤式 N 苯甲酰基 3 苯基异丝氨酸,四步反应总产率为28.4%。用IR、1HNMR、元素分析验证了化合物的结构。 相似文献
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N6-苯甲酰基-2',3'-O-异亚丙基-5'-(N-甲基-N-甲氧基酰胺)腺苷,Weinreb酰胺腺苷衍生物是用于制备Weinreb酮腺苷衍生物的重要中间体。报道了N6-苯甲酰基-2',3'-O-异亚丙基-5'-(N-甲基-N-甲氧基酰胺)腺苷的合成方法,以2',3'-O-异亚丙基腺苷为原料,经苯甲酰化、氧化反应和酰胺化反应,总收率为45%,其结构经1H NMR,13C NMR和HRMS表征。 相似文献
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1-苯基-3-甲基-4-咔唑-N-丁基-4-苯甲酰基呲唑啉-5-酮的合成及其光谱研究 总被引:4,自引:0,他引:4
在苯和50%NaOH介质中,80℃时1,4-二溴丁烷与咔唑(CZ)反应,生成N-溴丁基咔唑(BCZ)。在丙酮和K2CO2介质中,50℃时N-溴丁基咔唑与1-苯基-3-甲基-4-苯甲酰基吡唑啉-5-酮(PMBP)反应,生成1-苯基-3-甲基-4-咔唑-N-丁基-4-苯甲酰基吡唑啉-5-酮(PMCBP),详细研究了CZ,BCZ,PMBP和PMCBP的UV和IR光谱.在氯仿中PMCBP对Nd(Ⅲ)的萃取率是PMBP的2.3倍,PMBP-Nd(Ⅲ)配合物无荧光,但PMCBP-Nd(Ⅲ)配合物有很强的荧光,说明PM-CBP是Nd(Ⅲ)的优良荧光试剂。 相似文献
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以L-酪氨酸为起始原料,在碱性条件下与苯甲酰氯缩合得到N-苯甲酰基-O-苯甲酰基-L-酪氨酸(Ⅰ),收率87%;然后,在氯甲酸异丁酯-N-甲基吗啉(IBCF-NMM)的作用下与L-苯丙氨醇缩合形成具有双酰胺结构的N-(N-苯甲酰基-O-苯甲酰基-L-酪氨酰基)-L-苯丙氨醇(Ⅱ),收率80.7%;经碱水解得N-(N-苯甲酰基-L-酪氨酰基)-L-苯丙氨醇(Ⅲ),收率84.5%;在N,N-二甲基甲酰胺和无水K2CO3的作用下与二甲氨基氯乙烷盐酸盐反应4 h后得N-(N-苯甲酰基-O-二甲氨基乙基-L-酪氨酰基)-L-苯丙氨醇(Ⅳ),收率79%;最后,化合物Ⅳ在以1-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐(EDC.HCl)和4-二甲氨基吡啶(DMAP)为缩合剂的条件下与有机酸反应,合成了以苯丙二肽类化合物马蹄金素〔N-(N-苯甲酰基-L-苯丙氨酰基)-O-乙酰基-L-苯丙氨醇,MTS〕为先导化合物的衍生物共11个,其结构经NMR、ESI-MS进行了确认。 相似文献
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以4-甲氧羰基哌啶盐酸盐(1)和对三氟甲氧基苯甲酰氯(2)为起始原料,在三乙胺的作用下以92.7%的收率制得1-(4-三氟甲基苯甲酰基)-4-甲氧羰基哌啶(3);化合物(3)在羰基二咪唑与N,O-二甲基羟胺盐酸盐(4)作用下,以89.9%的收率制得1-(4-三氟甲氧基苯甲酰基)-4-(N-甲基-N-甲氧基羰基)哌啶(5);化合物(5)和4-甲氧基苯基溴化镁(6)偶联,以60.1%的收率制得化合物1-(4-三氟甲氧基苯甲酰基)-4-(4-甲氧基苯甲酰基)哌啶(7)。三步反应总收率50.0%。 相似文献
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[目的]寻找一条合成4-甲基-5-咪唑甲酸乙酯的新工艺路线。[方法]以乙酰乙酸乙酯、磺酰氯与甲酰胺为原料,采用一锅法合成一种用途广泛的多功能单体4-甲基-5-咪唑甲酸乙酯。[结果]通过实验,确定了一条合成4-甲基-5-咪唑甲酸乙酯的新工艺:以二氧六环为溶剂,环化时反应温度为120℃,反应时间为4 h,n(乙酰乙酸乙酯)∶n(磺酰氯)∶n(甲酰胺)为1∶1∶2,在该条件下,4-甲基-5-咪唑甲酸乙酯的产率为70%。[结论]该方法路线简单,原料易得,适合工业化生产。 相似文献
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β-氨基酸乙酯盐酸盐的合成与表征 总被引:1,自引:0,他引:1
以三种β-苯丙氨酸、二氯亚砜、乙醇为原料分别合成了β-苯丙氨酸乙酯盐酸盐、2F-β-苯丙氨酸乙酯盐酸盐和3F-β-苯丙氨酸乙酯盐酸盐三种稳定的β-氨基酸乙酯盐酸盐,并通过熔点、核磁和质谱对化合物的结构进行了表征。该合成方法操作简单、反应条件温和,收率均在85%以上。 相似文献
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在无水乙醇中,以二乙胺为催化剂,通过水杨醛与丙二酸二乙酯的Knoevenagel缩合反应合成了香豆素-3-羧酸乙酯,再经水解、酸化得到香豆索-3-羧酸。对影响香豆素-3-羧酸乙酯收率的原料配比、催化剂的用量进行了研究。所得最佳合成条件为:水杨醛与丙二酸二乙酯物质的量比1:1.2,二乙胺与水杨醛物质的量比为1:4,反应时间2h,在最佳工艺条件下。香豆素-3-羧酸乙酯的收率85%,香豆素-3-羧酸的收率95%。 相似文献
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Nicholas R. Krogman Arlin L. Weikel Nhu Q. Nguyen Katherine A. Kristhart Syam P. Nukavarapu Lakshmi S. Nair Cato T. Laurencin Harry R. Allcock 《应用聚合物科学杂志》2010,115(1):431-437
New biomedically erodible polymer composites were investigated. Polyphosphazenes containing the dipeptide side groups alanyl–glycine ethyl ester, valinyl–glycine ethyl ester, and phenylalanyl–glycine ethyl ester were blended with poly(lactide‐co‐glycolide) (PLGA) with lactic to glycolic acid ratios of 50 : 50 [PLGA (50 : 50)] and 85 : 15 [PLGA (85 : 15)] with solution‐phase techniques. Each dipeptide ethyl ester side group contains two N? H protons that are capable of hydrogen bonding with the carbonyl functions of PLGA. Polyphosphazenes that contain only the dipeptide ethyl ester groups are insoluble in organic solvents and are thus unsuitable for solution‐phase composite formation. To ensure solubility during and after synthesis, cosubstituted polymers with both dipeptide ethyl ester and glycine or alanine ethyl ester side groups were used. Solution casting or electrospinning was used to fabricate polymer blend matrices with different ratios of polyphosphazene to polyester, and their miscibilities were estimated with differential scanning calorimetry and scanning electron microscopy techniques. Polyphosphazenes with alanyl–glycine ethyl ester side groups plus the second cosubstituent were completely miscible with PLGA (50 : 50) and PLGA (85 : 15) when processed via solution‐casting techniques. This suggests that the hydrogen‐bonding protons in alanyl–glycine ethyl ester have access to the oxygen atoms of the carbonyl units in PLGA. However, when the same pair of polymers was electrospun from solution, the polymers proved to be immiscible. Solution‐cast miscible polymer blends were obtained from PLGA (50 : 50) plus the polyphosphazene that was cosubstituted with valinyl–glycine ethyl ester and glycine ethyl ester side groups. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 相似文献
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叙述了国内外N 苄基甘氨酸乙酯的几种化学制备方法,即分别以卤代乙酸乙酯、甘氨酸乙酯、叠氮乙酸乙酯和乙醛酸乙酯乙基半缩醛为起始原料的合成工艺。并介绍了N 苄基甘氨酸乙酯在农业、医药、化工等行业中合成有机中间体方面的应用情况。 相似文献
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Acer truncatum Bunge is a type of maple that is unique to China. Its fruit setting rate and seed oil content are both high. The oil is mainly composed of C16–C24 fatty acids and contains 5%–7% nervonic acid (NA). NA and its derivatives can delay ageing and prevent and treat disorders such as senile dementia and Alzheimer's disease. The content of NA ethyl ester prepared by the seed oil of A. truncatum Bunge is 5.84%. We report a new process for the enrichment of NA ethyl ester by urea inclusion (UI) and molecular distillation (MD), with the aim of obtaining highly pure NA ethyl ester. First, based on the difference in fatty acid ethyl ester saturation and carbon chain length, unwanted compounds such as oleic acid ethyl ester, linoleic acid ethyl ester, and sterol were removed by one-stage UI, the content of NA ethyl ester was increased to 18.69%. The oil in the UI compound was used as a feed, and differences in the mean molecular free paths between the components were exploited to separate the C16–C20 fatty acid ethyl esters (FAEEs) by two-stage MD. The total content of C16–C20 FAEEs decreased to 3.69% and the purity of NA ethyl ester increased to 47.47%. A new purification process of UI-MD-UI was established and NA ethyl ester could be purified to 91.8%. The combination of MD and UI has an important reference value for the industrialization of producing high-purity NA ethyl ester. 相似文献
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以氯化血红素(Ⅰ)为原料,经过脱铁、酯化、反马氏加成得到[2,7,12,18-四甲基-3,8-二(2-羟基乙基)-13,17-二甲氧基羰基乙基]-卟啉(异血卟啉二甲酯,Ⅳ)。在合成原卟啉二甲酯(Ⅲ)的过程中,采用了超声激励法,并且对反应条件进行了优化,产率达到91.6%;然后通过BH3-THF络合物同原卟啉二甲酯3,8-位乙烯基的反马氏加成合成了[2,7,12,18-四甲基-3,8-二(2-羟基乙基)-13,17-二甲氧基羰基乙基]-卟啉,并对加成体系进行适当优化,产率达到64.3%。通过1HNMR、MS、UV-vis和IR测试技术对产物结构进行了表征。 相似文献