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《高校化学工程学报》2021,(2)
为了解决N-(4-((1R,3S,5S)-3-氨基-5-甲基环己基)吡啶-3-基)-6-(2,6-二氟苯基)-5-氟吡啶酰胺(PIM447)中间体6-(2,6-二氟苯基)-5-氟吡啶-2-甲酸(化合物1)的放大工艺问题,以5-氟吡啶-2-甲酸(化合物2)为原料,经氧化、氯代、卤素交换、酯化、Suzuki偶联、水解反应制备了化合物1。化合物2与H2O2的氧化反应生成2-羧酸-5-氟吡啶-N-氧化物(化合物3)。化合物3与POCl_3氯代反应得到6-氯-5-氟吡啶-2-甲酸(化合物4),在HBr-HOAc溶液中,化合物4发生卤素交换反应得到6-溴-5-氟吡啶-2-甲酸(化合物5)。化合物5与MeOH酯化反应生成6-溴-5-氟吡啶-2-甲酸甲酯(化合物6)。化合物6与2,6-二氟苯硼酸发生Suzuki偶联反应得到6-(2,6-二氟苯基)-5-氟吡啶-2-甲酸甲酯(化合物7)。最后,化合物7在NaOH/MeOH溶液中水解生成目标化合物1,总收率达到58.7%。 相似文献
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以藜芦醛(Ⅰ)为起始原料,经过溴代、还原、傅克烷基化、脱甲基4步反应,合成了化合物4,5-二-(2-溴-4,5-二羟基苯甲基)-1,2-二苯酚(Ⅵ),总产率为53.5%。采用1HNMR、13CNMR、HREIMS等进行了结构表征。通过比色法对化合物Ⅵ及中间产物4,5-二-(2-溴-4,5-二甲氧基苯甲基)-1,2-二甲氧基苯(Ⅴ)进行蛋白酪氨酸磷酸酶1B(protein tyrosine phosphatase 1B,PTP1B)抑制活性测定,结果显示化合物质量浓度为20 mg/L时,化合物Ⅴ和Ⅵ的PTP1B酶抑制率分别为25.08%和79.48%,表明化合物Ⅵ具有较好的PTP1B酶抑制活性。 相似文献
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以邻甲酚、醋酸酐、4,4-二甲基异嗯唑-3-酮、4,6-二甲氧基-2-甲磺酰基嘧啶为原料,经乙酰化、溴化、Ⅳ_烷基化、醚化4步反应合成了标题化合物2-(2-(4,6-二甲氧基嘧啶-2-氧)苯基)-4,4-二甲基异嚷唑-3-酮,收率42.4%,化合物结构采用^1H NMR、IR、元素分析表征。 相似文献
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以3,5二-羟基苯乙酮(4)为原料,经三步反应制得3,5二-乙酰氧基苯乙烯(1)。在硫酸催化下化合物(4)与乙酸酐反应,得到3,5二-乙酰氧基苯乙酮(3),收率92%,对于化合物(3)进行了1H NMR表征;化合物(3)经催化加氢,得到1-(1羟-基乙基)-3,5二-乙酰氧基苯(2),收率98%,对于化合物(2)进行了1H NMR表征;化合物(2)在固体酸催化下反应得到3,5二-乙酰氧基苯乙烯(1),制备化合物(1)的反应条件为:m[化合物(2)]∶m(固体酸)=5∶1,110℃回流5 h,收率95%,纯度98%,对化合物(1)进行了IR,1H NMR,MS表征,并对化合物(1)的1HNMR,MS表征结果进行了进一步分析。 相似文献
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以2-氰基吡啶和水合肼为原料,经过Pinner反应和氧化反应合成得到3,6-二(吡啶-2-基)-1,2,4,5-四嗪(化合物1),收率为88.6%。对影响产物收率的因素进行了考察,确定了第二步氧化反应的反应温度为0℃,反应时间1.0h。化合物1分别与6,7-二溴-1,4-二氢-1,4-环氧萘(化合物4a)和6,7-二甲氧基-1,4-二氢-1,4-环氧萘(化合物4b)反应得到5,6-二溴异苯并呋喃(化合物5a)和5,6-二甲氧基异苯并呋喃(化合物5b)的收率分别为51.3%和48.5%。化合物1和化合物5a以及化合物5b的结构均采用~1H-NMR和ESI-MS进行了表征。 相似文献
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以3-氧代-4-甲酸甲酯四氢噻吩与氰化钠为原料,通过氰醇化、脱水、水解等反应合成了2,5-二氢噻吩-3,4-二羧酸酐(4),化合物4通过~1H NMR、~(13)C NMR、高分辨质谱(HRMS)等表征。研究了溶剂、反应温度以及不同配比的溶剂对合成2,5-二氢噻吩-3-4-二羧酸酐中间体的影响。制备3-氰基-4-甲酸甲酯-2,5-二氢噻吩(2)的较优条件为:POCl_3∶3-氰基-3-羟基-4-甲酸甲酯四氢噻吩(1)=2.5(物质的量比);制备2,5-二氢噻吩-3,4-二羧酸(3)的较优条件为:温度80℃,化合物2 1 g,乙酸2.9 mL,浓盐酸4.8 mL。对3-氰基-4-甲酸甲酯-2,5-二氢噻吩进行了~1H NMR、~(13) C NMR、HRMS表征。 相似文献
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对2,5-二甲基-3,4-二氢-4-氧代喹唑啉的合成进行了研究。以间甲基苯胺为原料经3步反应制得2-氨基-6-甲基苯甲酸,再环化生成2,5-二甲基-3,4-二氢-4-氧代喹唑啉。中间体及标题化合物结构经1 HNMR确证。 相似文献
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M. S. J. Simmonds W. M. Blaney F. Delle Monache M. Marquina Mac-Quhae G. B. Marini Bettolo 《Journal of chemical ecology》1985,11(12):1593-1599
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. 相似文献
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Cheng-Le Zhao Shane Porzio Alan Smith Haiyan Ge H. T. Davis L. E. Scriven 《Journal of Coatings Technology and Research》2006,3(2):109-115
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. 相似文献
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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. 相似文献
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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. 相似文献
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中蓝晨光化工研究院有限公司《塑料工业》编辑部 《塑料工业》2009,37(3)
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. 相似文献
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中蓝晨光化工研究院《塑料工业》编辑部 《塑料工业》2007,35(3):1-25,67
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。 相似文献