1,3,5-吡唑酮的制备工艺研究

本文以乙酰乙酸乙酯和苯肼为原料，通过环化、脱醇合成1，3，5-吡唑酮。探讨了合成反应的工艺条件，在最佳工艺条件下，产品的收率为95％，含量为99％。     

6-甲基-4-苯基-5-乙氧羰基-3,4-二氢嘧啶-2-硫酮的合成

利用Biginelli缩合反应,以苯甲醛、乙酰乙酸乙酯和硫脲为原料,合成了6-甲基-4-苯基-5-乙氧羰基-3,4-二氢嘧啶-2-硫酮。采用单因素法考察了催化剂种类、乙酰乙酸乙酯的用量、催化剂用量、反应时间、溶剂种类等对反应产率的影响。最佳反应条件为:以0.10g氨基磺酸作催化剂,以10mL无水乙醇为溶剂,以10mmol苯甲醛、24mmol乙酰乙酸乙酯和15mmol硫脲为原料,在搅拌回流条件下反应3h。产率为79.0%。     

1-苯基-3-甲基-5-氯-4-吡唑甲酸的合成研究

含有吡唑环的化合物具有广泛的生物活性。1-苯基-3-甲基-5-氯-4-吡唑甲酸是吡唑类化合物的重要中间体,以苯肼和乙酰乙酸乙酯为起始原料,以苯肼和乙酰乙酸乙酯为原料,经过环合反应、Vilsmeier-Haack反应、氧化反应,三步收率分别为85%、80%、80%。环合反应、Vilsmeier-Haack反应进行了正交实验,得到较佳的反应条件。     

3-甲基-5-吡唑酮的合成研究

采用乙酰乙酸乙酯和水合肼为原料 ,无水乙醇为溶剂 ,对 3-甲基 - 5 -吡唑酮的合成反应进行了研究 ,在反应温度为 80°C,乙酰乙酸乙酯与水合肼摩尔比为 1∶ 1 .2 ,反应时间 3h的较佳工艺条件下 ,产物收率大于 85 % ,产物纯度大于 99.5 %。用 IR光谱对产物结构进行了确认     

7-羟基-4-甲基香豆素的合成

研究了间苯二酚和乙酰乙酸乙酯合成7-羟基-4-甲基香豆素，考察了影响反应的主要因素。反应的最优条件：反应温度为75℃，对甲苯磺酸0．5g，间苯二酚0．1mol，a(间苯二酚)：n(乙酰乙酸乙酯)为1．0：1．0，反应时间为2h，在此条件下产率为91．8％。     

5-二氟甲基-1-取代苯基-1H-吡唑-4-甲酰肼的合成

以取代苯肼盐酸盐和二氟乙酰乙酸乙酯为原料经缩合、成环、肼解,得到了7个结构全新吡唑酰肼类化合物,所有化合物经核磁氢谱、碳谱和高分辨质谱确证。对成环反应条件进行了研究,取代苯肼盐酸盐中和后进行反应为宜,并且其水分含量是影响反应的关键因素。     

显影剂4-甲基-1-苯基-3-吡唑酮的合成

以苯肼与甲基丙烯酸甲酯为原料，在乙醇钠存在下通过缩合反应制备4-甲基-1-苯基-3-吡唑酮，探讨了合成反应的工艺条件。在最佳工艺条件下，产品的收率平均为93．3％，纯度达99．5％。     

4-甲基-2-乙基-6-羟基嘧啶的合成研究

以丙腈为原料，与氯化氢、氨气反应合成丙眯盐酸盐，在水溶液中同乙酰乙酸乙酯反应合成4-甲基-2-乙基-6-羟基嘧啶。考察了反应时间、反应温度、物料配比、pH值对4-甲基-2-乙基-6-羟基嘧啶收率的影响。优化条件为：反应温度40℃、反应的pH=12．4、反应时间为6～7h、乙酰乙酸乙酯与丙腈的物质的量比为1．09：1．0，在此条件下反应的总收率为88．7％。     

2，4-二氯-5-异丙氧基苯肼的合成

研究了以2，4-二氯-5-异丙氧基苯胺为原料，经重氮、碱解合成2，4-二氯-5-异丙氧基苯肼的工艺，讨论了反应条件对反应的影响，获得了较好的工艺条件。在优化条件下二步反应总收率达到91％(以2，4-二氯-5-异丙氧基苯肼计)。产品是合成农药口恶草酮的重要中间体。     

4-（4-二甲氨基）苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2-酮的合成

采用氨基磺酸作催化剂,无水乙醇作溶剂,对二甲氨基苯甲醛、乙酰乙酸乙酯和脲在加热搅拌条件下回流反应3 h,合成了4-（4-二甲氨基）苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2-酮,产率为78.5%。     

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.     

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.     

Methyl 2,4,6-decatrienoates Attract Stink Bugs and Tachinid Parasitoids

Halyomorpha halys (Stål) (Pentatomidae), called the brown marmorated stink bug (BMSB), is a newly invasive species in the eastern USA that is rapidly spreading from the original point of establishment in Allentown, PA. In its native range, the BMSB is reportedly attracted to methyl (E,E,Z)-2,4,6-decatrienoate, the male-produced pheromone of another pentatomid common in eastern Asia, Plautia stali Scott. In North America, Thyanta spp. are the only pentatomids known to produce methyl 2,4,6-decatrienoate [the (E,Z,Z)-isomer] as part of their pheromones. Methyl 2,4,6-decatrienoates were field-tested in Maryland to monitor the spread of the BMSB and to explore the possibility that Thyanta spp. are an alternate host for parasitic tachinid flies that use stink bug pheromones as host-finding kairomones. Here we report the first captures of adult and nymph BMSBs in traps baited with methyl (E,E,Z)-2,4,6-decatrienoate in central Maryland and present data verifying that the tachinid, Euclytia flava (Townsend), exploits methyl (E,Z,Z)-2,4,6-decatrienoate as a kairomone. We also report the unexpected finding that various isomers of methyl 2,4,6-decatrienoate attract Acrosternum hilare (Say), although this bug apparently does not produce methyl decatrienoates. Other stink bugs and tachinids native to North America were also attracted to methyl 2,4,6-decatrienoates. These data indicate there are Heteroptera in North America in addition to Thyanta spp. that probably use methyl 2,4,6-decatrienoates as pheromones. The evidence that some pentatomids exploit the pheromones of other true bugs as kairomones to find food or to congregate as a passive defense against tachinid parasitism is discussed.     

2005～2006年国外塑料工业进展

收集了2005年7月～2006年6月国外塑料工业的相关资料，介绍了2005—2006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生产量以及各国塑料制品的进出口情况。作为对比，介绍了中国塑料的生产情况。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（聚酰胺、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚）、通用热固性树脂（酚醛、聚氨酯、不饱和树脂、环氧树脂）、特种工程塑料（聚苯硫醚、液晶聚合物、聚醚醚酮）的品种顺序，对树脂的产量、消费量、供需状况及合成工艺、产品开发、树脂品种的延伸及应用的扩展作了详细的介绍。     

2007～2008年世界塑料工业进展

收集了2007年7月～2008年6月世界塑料工业的相关资料,介绍了2007～2008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、不饱和聚酯树脂、环氧树脂)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.