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研究了以硝基甲烷和二硫化碳为原料,合成1,1-二甲硫基-2-硝基乙烯。考察了反应温度、反应时间、甲基化试剂、溶剂、投料比等对于反应产物的影响,得到优化工艺条件为:反应温度35℃,反应时间3h。以硫酸二甲酯为甲基化试剂,常温下反应时间3 h,重结晶得1,1-二甲硫基-2-硝基乙烯,收率为84%,产物通过IR、1H-NMR鉴定。 相似文献
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以芴、多聚甲醛和乙醇钠等为主要原料,经过醚化、酯化和Friedel—Crafts酰基化等反应,合成了9,9-双羟甲基芴(BHMF)、9,9-双甲氧甲基芴(BMF)、丁二酸单乙酯和丁二酸单乙酯酰氯(ESC)这4种中间体,最终合成出目的产物2-丁二酸单乙酯酰基-9,9-双甲氧甲基芴,利用傅立叶红外光谱对中间体和目的产物结构进行了分析和表征。 相似文献
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以邻苯二胺和丙二酸为原料,在3 mol/L盐酸催化下合成双(1H-苯并咪唑-2-基)甲烷中间体,然后与月桂醛通过Knoevenagel缩合反应合成了双苯并咪唑衍生物——1,1-双(1H-苯并咪唑-2-基)-1-十三碳烯。利用元素分析、FTIR和~1HNMR对合成产物的结构进行了表征,考察了常规碱催化剂对目标产物收率的影响,并通过UVVis和荧光光谱(FL)测定了目标化合物的光学性能。结果表明:六氢吡啶催化效果最好,产物收率可达76.33%。目标化合物在243、315和361 nm 3处有紫外吸收峰,可有效覆盖日光紫外线UVA和UVB波段;目标化合物溶液在λem=464.5 nm处有蓝紫色荧光,固体薄膜在λ_(em)=476.5 nm处有蓝紫色荧光,荧光量子产率为0.47。标题化合物荧光增白效果与常用荧光增白剂VBL相当。 相似文献
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Summary Poly(2,5-(3,4-bis(methoxymethyl)furanylene)vinylene)s of various microstructures, prepared by aqueous Ring Opening Metathesis Polymerisation (ROMP) of exo,exo-5,6-bis(methoxymethyl)-7-oxabicylo[2.2.1]hept-2-ene, were characterised by high field NMR. 相似文献
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报道了一种合成(S)-2-羟甲基氮杂环丁烷的新方法,即以γ-丁内酯为起始原料,经溴代开环成2,4-二溴丁酸甲酯(■),然后与(S)-α-苯乙胺双取代环化生成氮杂1-[(S)-1-苯乙基]-2-甲氧羰基氮杂环丁烷的两种非对映异构体■(2S,1′S)和■(2R,1′S),经柱层析分离,氢化铝锂还原成醇(■)后,氢解脱去(S)-1-苯乙基和引入Boc保护基生成标题化合物1-叔丁氧羰基-(S)-2-羟甲基氮杂环丁烷。总共4步反应,总收率为40%。~1H NMR和MS表征确证了关键中间体和目标产物结构。 相似文献
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Summary Living poly(tetrahydrofuran) (PTHF) was coupled with sodium p-vinylbenzyloxide quantitatively to prepare a macromer of p-vinylbenzyloxyl poly(tetrahydrofuran) (VBO-PTHF). The radical polymerization of the macromer with AIBN was performed. From the GPC measurement the conversion of the macromer to poly-macromer was shown to be high percentage, but the degree of polymerization of poly-macromer was much lower than that expected in the case of regular monomers such as styrene. 相似文献
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A series of 1,4-distyrylbenzene derivatives containing 1,1-dicyanovinyl moieties were designed as poly-p-phenylenevinylene analogs to obtain the red electroluminescence assisted by the computational results. Based on the subsequent synthesis and optical studies, the present work indicated that introduction of 1,1-dicyano group as electron receptor in PPV skeleton could shift the electroluminescence significantly to the red region. The present work has shown a successful strategy to tune the emission of PPV analogs based on the theoretical design and organic synthesis. 相似文献
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John M. Geurts Christianne M. Gttgens Marco A. I. Van Graefschepe Rob W. A. Welland J. J. G. Steven Van Es Anton L. German 《应用聚合物科学杂志》2001,80(9):1401-1415
For use in emulsion and solution copolymerization a series of novel amino‐functional methacrylates has been synthesized, most of which have seldom, or never, been described in the literature before. In this investigation, the preparation of the hydrochloric and/or tosylate salt of the monomers aminoethyl, 3‐amino‐1‐propyl, 5‐amino‐1‐pentyl, 6‐amino‐1‐hexyl and 11‐amino‐1‐undecyl methacrylate will be described, along with the characterization of the parameters water solubility, pKa and chemical stability. The homopolymers of these monomers have been prepared and characterized. Results show the occurrence of an acyl migration upon neutralization of the monomers aminoethyl‐ and 3‐amino‐1‐propyl methacrylate. This migration does not occur in the monomer 5‐amino‐1‐pentyl methacrylate, which makes it possible to synthesize the neutralized monomer although, after neutralization, a Michael addition occurs, resulting in a limited lifetime. Copolymerizations have been performed in emulsion. The monomer aminopentyl methacrylate especially proved to be suitable for emulsion copolymerizations when used under controlled conditions. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 1401–1415, 2001 相似文献
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Electrochemical Carboxylation of Cinnamoyl-1,1-bis(alkylthio)ethylenes Cinnamoyl-1,1-bis(alkylthio)ethylenes ( 1a–1h ) are reduced electrochemically in the presence of carbondioxide in aprotic media. The attack of CO2 takes place either in 1- or 5-position of cinnamoyl-1, 1-bis(alkylthio)ethylenes ( 1a–1h ) depending on the nature of the aryl substituents. If CO2 reacts in position 1 carbonic acids 3 are obtained, reaction of carbondioxide in 5- position leads to the acids 2 . The effects of different aryl substituents on the halfwave potentials and the preparative electrolyses have been investigated. 相似文献