两个Ga环五肽类似物的合成及研究

本文以Leu和Phe为起始原料,改变其环合位点,优化其合成路线,合成了两个GA类似物,其环合收率达近50%。使用反相HPLC进行分离纯化,通过1H-NMR、13C-NMR和MS对其结构进行表征。     

两个Galaxamide环五肽类似物的合成

以亮氨酸和苯丙氨酸为起始原料,改变其环合位点,优化其合成路线,合成了两个Galaxamide环五肽类似物,其环合收率近50%。使用反相HPLC进行分离纯化,通过1HNMR、13CNMR和MS对其结构进行表征。     

吡啶环化合物的合成与结构表征

以2,6-二甲基吡啶、正丁基锂为初始原料,在温和的条件下,经1倍正丁基锂去氢后与苯乙酮加成得到含N,O-二齿配体化合物[2-(6-(CH3)C5H4N)CH2C(OH)(Ph)CH3],应用1 H NMR技术对其进行了结构表征。     

天然五肽L-Tyr-Pro-Ile-Pro-Phe-OH的全合成

针对目标物的结构特征,运用反合成设计,将其切为2个合成片断:Boc-L-Tyr-Pro-OH(片段A)和L-Ile-Pro-Phe-OMe (片段B),先合成2个片断,然后将2个片断连接后去保护,完成了标题化合物的全合成,总收率48.08%.关键中间体与最终产物的化学结构经1HNMR、13CNMR、IR、MS-ESI和HPLC等表征及分析予以确认.     

固相合成胸腺五肽的分离与纯化

胸腺五肽(TP5)是一种很有发展前景的药物,具有胸腺素的全部生理功能。固相合成法是胸腺五肽生产的主流技术,目前,对固相合成的五肽一般采用反相色谱技术纯化,但效率低、成本高,仅限于小规模制备。实验采用离子交换法纯化,并进行了方案优化,发现在pH4 4醋酸盐缓冲液平衡、盐梯度洗脱条件下纯化TP5,一步分离纯度可达98 23%。该法可以满足大规模制备的要求,且成本很低。     

磷杂螺环化合物的合成及表征

合成了双（４ 甲撑 ２，６，７ 三氧杂 １ 磷杂双环［２，２，２］辛烷）磷酸三聚氰胺盐（Ⅲ）及２，６，７ 三氧杂 １ 磷杂双环［２，２，２］辛烷甲醇（Ⅰ）、双（４ 甲撑 ２，６，７ 三氧杂 １ 磷杂双环［２，２，２］辛烷）氯代磷酸酯（Ⅱ），三者的得率分别为７２７％、９００％及５７３％；同时对化合物（Ⅰ）、（Ⅱ）及（Ⅲ）的核磁共振碳谱和红外光谱谱图进行了归属和解析，并得到元素分析的证实     

一个芳环堆积共结晶化合物的合成与表征

在溶剂中,采用水热法合成得到了一个共结晶的芳环堆积化合物C_8H_5O_7S·C_(10)H_9N_2·(C_(10)H_8N_2)_(0.5)(C_(10)H_8N_2=2,2’-联吡啶)。采用X射线单晶衍射和元素分析对其结构和组成进行了表征。X射线单晶衍射表征结果表明,该化合物晶体属于三斜晶系。研究了该化合物的荧光光谱以及热稳定性,该化合物荧光发射峰在417nm,热稳定性较好。     

3-氧环丁羧酸的合成研究

以丙酮、甲醇、溴和丙二酸二酯为起始原料,经过溴化、环合、水解及脱酸合成了3-氧环丁羧酸,4步反应总收率44.07%。产品经1H NMR、元素分析和质谱表征。改进后的方法具有操作简单、成本低等优点,适合工业化生产。     

新型手性大环多胺化合物的合成及表征

以2,5-二甲基吡嗪为原料合成吡嗪-2,5-甲醛,再通过与1R,2R-环己二胺合成一种新型的手性大环多胺类化合物L,通过1H NMR、FT-IR对所合成的物质的结构进行了表征。     

卟啉化合物的合成

卟啉化合物广泛存在于自然界中和生命体中,对生命活动起着重要作用,卟啉化合物因其特殊的结构和生物活性,应用前景广阔。本文主要介绍卟啉化合物的合成方法,根据所采用起始反应物的不同,将卟啉的合成方法分为两大类：全合成法和半合成法,对两类合成方法给予较详细的介绍。     

Synthesis and design of new hybrid configurations for biobutanol purification

The development of new technologies for biobutanol production by fermentation has resulted in higher butanol concentrations, less by-products and higher volumetric productivities during fermentation. These new technology developments have the potential to provide a production process that is economically viable in comparison to the petrochemical pathway for butanol production. New alternative hybrid configurations based on liquid–liquid extraction and distillation for the biobutanol purification were presented. The alternatives are designed and optimized minimizing two objective functions: the total annual cost (TAC) as an economical index and the eco-indicator 99 as an environmental function. All the new configurations presented reduced the TAC compared to the traditional hybrid configuration, in particular a thermally coupled alternative exhibited a 24.5% reduction of the TAC together with a 11.8% reduction of the environmental indicator. Also intensified sequences represented a promising option in the reduction of the TAC but with some penalty in the eco-indicator.     

一种环状膦酸酯的合成及其结构表征

合成了一种环状膦酸酯DMDP,用元素分析、红外、1HNMR分析方法表征了其组成和结构,解释了其谱图现象。     

Synthesis and properties of new aromatic copolyesters containing phosphorous cyclic bulky groups

A series of phosphorus‐containing copolyesters was prepared by polycondensation of 2‐(6‐oxido‐6H‐dibenz<c,e><1,2>oxaphosphorin‐6‐yl)‐1,4‐naphthalene diol, 1 , or of an equimolecular amount of 1 and different bisphenols 2 , such as 4,4′‐isopropylidenediphenol, 4,4′‐(hexafluoroisopropylidene)diphenol and 2,7‐dihydroxynaphthalene, with an aromatic diacid chloride containing two preformed ester groups 3 , namely, terephthaloyl‐bis‐(4‐oxybenzoyl‐chloride). The copolyesters exhibited good thermal stability having the temperature of 5% weight loss above 380°C and char yield at 700°C in the range of 20–31.2%. The glass transition temperature was in the range of 136–147°C. The polymers exhibited thermotropic liquid crystalline behavior, as was observed with polarized optical microscopy, differential scanning calorimetry, and X‐ray experiments. POLYM. ENG. SCI., 2010. © 2010 Society of Plastics Engineers     

A potent integrin antagonist from a small library of cyclic RGD pentapeptide mimics including benzyl-substituted azabicycloalkane amino acids

A small library of cyclic RGD pentapeptide mimics, including benzyl-substituted azabicycloalkane amino acids, was synthesized with the aim of developing active and selective integrin antagonists. In vitro binding assays established one particular compound with affinity for both the alpha(v)beta(3) and the alpha(v)beta(5) integrins. The synthesis in solution and the in vitro screening of these RGD derivatives, as well as the determination of the conformational properties of the integrin ligands by spectroscopic and computational methods are described.     

Synthesis and purification of anthraquinone in a multifunctional reactor

In the present paper the reaction of 2-benzoylbenzoic acid dehydration has been studied in the presence of different catalysts by using a batch reactor for screening the best catalysts and a pseudo-continuous multifunctional reactor for determining catalysts productivity, reaction yields, catalysts deactivation and regeneration on the previously selected catalysts that are acid bentonite, Y- and β-zeolites. This last reactor works also as evaporator and condenser for separating and collecting produced anthraquinone at a high level of purity, while water continuously formed evaporates in the atmosphere.

A kinetic model with vapour–liquid partition and catalyst deactivation has been used to interpret the experimental runs. The liquid reacting mixture showed strong non-ideality favouring the evaporation and collection of pure anthraquinone.     

N-乙烯基己内酰胺的合成工艺改进与产品纯化

用乙炔作乙烯化剂,高压法合成出标题化合物,最佳工艺条件优化:在放大时最佳的脱水条件是加入溶剂比为1.0∶0.2;在反应温度90～120℃,反应时间8.0～9.0h,压力1.0～2.0MPa;以水作结晶溶剂,水的用量比例最低为1.0∶1.0;用气相色谱-质谱联用仪(GC/MS)和红外光谱检测表明,简单蒸馏得到w(NVCL)=92%～96%(气相色谱GC)的样品,经进一步精馏分离可得到质量分数99%(GC)以上的NVCL产品。     

乙交酯的合成及纯化

以煤法制乙二醇（EG）工艺中的副产物羟基乙酸为原料,先预聚成低分子量聚羟基乙酸再解聚制备乙交酯。研究发现解聚升温速率对乙交酯的收率具有重要影响,同时考察了各反应条件对乙交酯收率的影响。结果表明：在聚合温度180℃,加入催化剂Sb2O3量为0.75wt%, 以15℃/min的速率升至290℃有最佳解聚效果,粗产物乙交酯的收率高达87.5%,三次重结晶后纯度高于99.9%,收率为78.0%,并通过红外光谱、核磁共振氢谱等对产物乙交酯进行了表征。     

一种新型石油净化系统研制

提出了一种新型高效石油过滤与净化系统.系统由两台过滤罐组成,每台过滤罐均可处理100%流量的原料油,正常操作情况下,每个过滤罐将高效地反复执行如下4个工序填充工序、过滤工序、反洗工序、浸泡工序.系统以稳定的可编程控制器为控制核心,以触摸屏为人机交互接口,编程开发智能化控制软件,通过内置容错处理模块,保证了系统的安全稳定运行.系统能低耗、高效地实现了石油净化处理,原油净化效率高,出油质量提高显著.     

新星色剂二溴对甲基偶氮羧胂的合成、纯化及其反应特性

设计、合成了一组新的不对称变色酸双偶氮羧胂类试剂。研究了共与铋、稀土、钍的显色反应性能，并对其进行了提纯鉴定。确定了其组成及结构。实验证明新试剂可成为铋和铈组稀土的优良显色剂。