2-氨基苯甲醇N-烷基化合成N-(芳甲基)-2-((2-羟甲基苯基)氨基)乙酰胺

基于溴苄与2-氨基苯甲醇的N-烷基化反应制备2-(苄基氨基)苯基甲醇的条件进行了优化探究。利用单因素法,探讨了反应溶剂、碱的种类及用量、反应温度、时间、物料比等对反应的影响,并通过正交实验法获得影响反应因素的顺序为:原料比反应温度反应时间碱的用量,从而优化了反应条件。在优化条件下,合成了一系列N-(芳甲基)-2-(2-羟甲基苯基氨基)乙酰胺类化合物,收率为58%～69%。     

3-乙酰基-2-氯吲哚中氨基的烷基化和苄基化保护研究

以3-乙酰基-2-氯吲哚为原料,在丙酮的碱性溶液中发生烷基化和苄基化反应对氨基进行保护。探讨了反应温度及溶剂对反应产率的影响,在优化的反应条件下以良好到优异的产率(78.5%～97.7%)合成了N-烷基或苄基取代-3-乙酰基-2-氯吲哚。它们的结构通过红外光谱、核磁共振氢谱、质谱以及元素分析得以证实。     

3-硝基-2-氨基吡啶和5-硝基-2-氨基吡啶的制备

研究了以2-氨基吡啶为原料,经氨基N-硝化、酸性重排获得3-硝基-2-氨基吡啶和5-硝基-2-氨基吡啶后,应用减压水蒸气蒸馏的办法分离得到两种纯化合物。对反应条件和两种异构体之间的比例进行了研究。     

4-苄基-2-羟基-吗啉-3-酮的合成

以乙醛酸和N-苄基乙醇胺为原料,合成4-苄基-2-羟基-吗啉-3-酮。通过正交实验考察了反应条件对目标产物收率的影响。结果表明,当原料摩尔比n(乙醛酸)∶n(N-苄基乙醇胺)=2∶1,反应时间22 h,反应溶剂四氢呋喃用量35 mL,反应温度65℃时,目标产物的收率最高可达62%。并进一步考察了反应温度和原料摩尔比对反应收率的影响。     

4-氨基-5-(3,4,5-三甲氧基苄基)嘧啶-2-醇的合成

以化合物3-苯基氨基-2-(3,4,5-三甲氧基苄基)丙烯腈为主要原料,以甲醇钠为缩合剂,与尿素反应得目标化合物4-氨基-5-(3,4,5-三甲氧基苄基)嘧啶-2-醇,反应收率达到76.3%。经HPLC检测,纯度达98.6%。用FT-IR、1HNMR和元素分析对目标化合物的结构进行了表征。     

3-氨基吡咯烷及其N-衍生物的合成

3-氨基吡咯烷的二盐酸盐和乙酰化物是合成托氟沙星和其它喹诺酮类抗菌药的关键中问体。以苄胺和丙烯酸乙酯为原料经加成反应制得3-苄胺基丙酸乙酯：再与氯乙酸甲酯进行N-烷基化反应制得3-[N-(甲氧羰基亚甲基)苄胺基]丙酸乙酯；然后经狄克曼缩合、脱羧而得1-苄基-3-吡咯烷酮：再经肟化、还原而得中间体3-氨基-1-苄基吡咯烷，并由它进而制得目标化合物的路线因原料价廉易得而具有很大的工业化价值。但原有方法存在产率低，操作烦琐等缺点。经过研究，将原来的N-烷基化反应收率从62．4％提高到95％以上，并对其它一些反应操作进行了相应改进：从而得到一条原料价廉易得，操作方便，成本低的适于工业化的制备目标产物的工艺路线。     

2-(N-4-甲基苄基)甲氧乙酰氨基异丁酸甲酯的合成方法

正本发明公开了一种2-(N-4-甲基苄基)甲氧乙酰氨基异丁酸甲酯的合成方法,其特点是该方法将对甲基亚苄氨基乙酸甲酯与N,N-二甲基甲酰胺和四正丁基碘化铵混合,在常压下饱和二氧化碳后以恒电流电羧化反应,经酯化后提纯得2-(N-4-甲基苄基)甲氧乙酰氨基异丁酸甲酯。本发明与现有技术相比具有工艺简单,操作方     

放射性^99mTc标记的NMDA受体配基N2S2-Memantine的合成

以美金刚胺为原料,先与氯乙酰氯反应,再与二硫二氮缩合,最后与醋酸汞硫化氢反应脱巯基保护基得到标记前体N-[2-(N-(2-巯基乙基))氨基甲酰甲基J-N-(2-巯基乙基)-3,5-二甲基金刚烷胺基乙酰胺.关键化合物N-[2-((2-(S-(4-甲氧基苄基)巯基)乙基)氨基)乙酰基]-S-(4-甲氧基苄基)-2-氨基乙硫醇和N-[2-(S-(4-甲氧基苄基)硫基)乙基]-N-[N-(2-(S-(4-甲氧基苄基)硫基)乙基)氨基)甲酰甲基]-3,5-二甲基金刚烷胺基乙酰胺得到核磁和质谱表征,总收率为32%.     

BF_3·OEt_2催化合成1-(酰胺苄基)-2-芳基-3,1-苯并噁嗪类化合物

在BF_3·OEt_2的催化作用下, N-苄基-2-(2-羟甲基苯基氨基)乙酰胺与硝基苯甲醛反应合成了1-酰胺基苄基-2-芳基-3,1-苯并噁嗪。研究了催化剂对反应的影响,实验结果表明BF_3·OEt_2比TMSCl, pTsOH, ZnCl_2和FeCl_3对反应的催化活性高。     

4-(2-乙酰氨基-3-羧基丙酰氨基)苯甲酸的合成工艺研究

以L-天冬氨酸和乙酸酐为原料,经脱水环化合成N-乙酰-L-天冬酸酐,然后与对氨基苯甲酸经N-酰化反应合成得到新化合物4-(2-乙酰氨基-3-羧基丙酰氨基)苯甲酸。通过Scifinder查询,未发现它的报道。研究了物料配比、反应温度、反应时间和溶剂等因素对产物收率的影响。优化条件为:无水乙醇作溶剂,n(N-乙酰-L-天冬酸酐)∶n(对氨基苯甲酸)=1∶1,反应温度为45℃,反应时间为3 h。优化条件下产物收率为78.7%。目标化合物经熔点、红外和核磁氢谱确证。     

Sapindaceae,cyanolipids, and bugs

Scentless plant bugs (Heteroptera: Rhopalidae) are so named because adults of the Serinethinae have vestigial metathoracic scent glands. Serinethines are seed predators of Sapindales, especially Sapindaceae that produce toxic cyanolipids. In two serinethine species whose ranges extend into the southern United States,Jadera haematoloma andJ. sanguinolenta, sequestration of host cyanolipids as glucosides renders these gregarious, aposematic insects unpalatable to a variety of predators. The blood glucoside profile and cyanogenesis ofJadera varies depending on the cyanolipid chemistry of hosts, and adults and larvae fed golden rain tree seeds (Koelreuteria paniculata) excrete the volatile lactone, 4-methyl-2(5H)-furanone, to which they are attracted.Jadera fed balloon vine seeds (Cardiospermum spp.) do not excrete the attractive lactone. Loss of the usual heteropteran defensive glands in serinethines may have coevolved with host specificity on toxic plants, and the orientation ofJadera to a volatile excretory product could be an adaptive response to save time.Mention of a commercial product does not consititute an endorsement by the USDA.     

2008～2009年世界塑料工业进展

收集了2008年7月～2009年6月世界塑料工业的相关资料,介绍了2008～2009年国外塑料工业的发展情况,提供了世界塑料产量、消费量及全球各类树脂的需求量及产能情况。按通用热塑性树脂(聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂)、工程塑料(尼龙、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚)、特种工程塑料(聚苯硫醚、液晶聚合物、聚醚醚酮)、通用热固性树脂(酚醛、聚氨酯、环氧树脂、不饱和聚酯树脂)不同品种的顺序,对树脂的产量、消费量、供需状况及合成工艺、产品应用开发、树脂品种的延伸及应用的进一步扩展等技术作了详细介绍。     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Many Drugs of Abuse May Be Acutely Transformed to Dopamine,Norepinephrine and Epinephrine In Vivo

It is well established that a wide range of drugs of abuse acutely boost the signaling of the sympathetic nervous system and the hypothalamic–pituitary–adrenal (HPA) axis, where norepinephrine and epinephrine are major output molecules. This stimulatory effect is accompanied by such symptoms as elevated heart rate and blood pressure, more rapid breathing, increased body temperature and sweating, and pupillary dilation, as well as the intoxicating or euphoric subjective properties of the drug. While many drugs of abuse are thought to achieve their intoxicating effects by modulating the monoaminergic neurotransmitter systems (i.e., serotonin, norepinephrine, dopamine) by binding to these receptors or otherwise affecting their synaptic signaling, this paper puts forth the hypothesis that many of these drugs are actually acutely converted to catecholamines (dopamine, norepinephrine, epinephrine) in vivo, in addition to transformation to their known metabolites. In this manner, a range of stimulants, opioids, and psychedelics (as well as alcohol) may partially achieve their intoxicating properties, as well as side effects, due to this putative transformation to catecholamines. If this hypothesis is correct, it would alter our understanding of the basic biosynthetic pathways for generating these important signaling molecules, while also modifying our view of the neural substrates underlying substance abuse and dependence, including psychological stress-induced relapse. Importantly, there is a direct way to test the overarching hypothesis: administer (either centrally or peripherally) stable isotope versions of these drugs to model organisms such as rodents (or even to humans) and then use liquid chromatography-mass spectrometry to determine if the labeled drug is converted to labeled catecholamines in brain, blood plasma, or urine samples.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.