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丙腈

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The epoxidation of of various olefins was carried out using LDH-F with Mg/Al=5 as the catalyst and H2O2 and benzonitrile as the oxidants. This catalytic system has excellent catalytic activity. The conversion and selectivity are both above 95% when using styrene, indene, allyl alcohol, and allyl chloride as the substrates.

以Mg/Al=5的LDH-F为催化剂,H2O2和苯甲腈为氧化剂对不同官能团化烯烃进行环氧化反应,结果表明,此催化体系具有良好的催化性能,在苯乙烯、茚、丙烯醇和烯丙基氯环氧化反应中转化率和选择性均在95%以上。

Methods: The analytical column was SHIMADZU VP-ODS C18 column(4.6 mm×150 mm 5 μm) with a mobile phase consisted of 0.05 mol/L disodium hydrogen phosphate solution(85% phosphoric acid solution with pH adjustment to 2.5)-acetonitrile-methanol(42.5∶47.5∶10) at the flow rate of 1.0 ml/min the detection wavelength was set at 254 nm.

目的:建立丙酸氯倍他索尿素乳膏中丙酸氯倍他索含量的HPLC测定方法。方法:色谱柱为SHIMADZU VP-ODS C18柱(4.6 mm×150 mm5 μm)流动相为0.05 mol/L磷酸氢二钠溶液(用85%磷酸溶液调节pH值至2.5)-乙腈-甲醇(42.5∶47.5∶10)流速为1.0 ml/min 检测波长为254 nm。

The experimental results show that using the feed technique of "starved state" can raise the conversion ratio of monomers, shorten the reactive time and get polymers with much more even distribution of molecular weight; the technique of adding azobisisobutyronitrile as an initiator first and then benzoperoxide as another initiator at later Stage of experiment can get higher initiating efficiency than using one initiator only.

结果表明:采用&饥饿态&聚合工艺可提高单体转化率,缩短反应时间,且所得到聚合物相对分子质量分布均匀;选用偶氮二异丁腈和过氧化笨甲酰两种引发剂进行复配,比选用单一引发剂的引发效果好;选用酯酸丁酯、正丁醇和丙二醇甲醚丙酸酯作混合溶剂,当配比为2:1:1时聚合体系稳定,聚合物的固体质量分数可达70%,且粘度适中。

In chapter four, the preperation of ytterbium diiodide was examined. The reductive cleavage of Se-Se bond and S-S bond induced by ytterbium diiodide was investigated. The reaction of diselenides and disulfides with allylic bromide promoted by ytterbium diiodide was also examined. The intermolecular Barbier-type reaction induced by ytterbium diiodide was studied. In the last section of this chapter, the intermolecular reductive coupling of nitriles with azides induced by samarium diiodide was investigated.

第四章,研究了二碘化镱的制备方法,以及二碘化镱作为一种优良的单电子转移试剂在有机合成中的应用:二硒醚的Se--Se键和二硫醚S-S键的还原断裂,及其在合成烯丙基硒醚,硒代酯和烯丙基硫醚,硫代酯中的应用,实验结果表明二碘化镱也能促进分子间的Barbier反应,而文献认为二碘化镱不能促进分子间的Barbier反应;最后研究了二碘化钐促进的叠氮化合物与腈的交叉还原偶联反应,一步高收率地制备脒的方法。

Thirdly, The preparation of 3-aryl-5-substituted-ethenyl isoxazoles and l-isoxazolyl-2-isoxazolinyl substituted-ethenes was developed through 1, 3-dipolar cycloaddition of nitrile oxides,α-alkylation reaction and another 1, 3-dipolar cycloaddition of nitrile oxides based on polystyrene-supported propargyl selenide.

三、从聚苯乙烯负载的炔丙基硒醚出发,经过腈氧化物的1,3-偶极环加成反应、α-烷基化反应和腈氧化物的1,3-偶极环加成反应固相分别合成了3-芳基5-取代--乙烯基异噁唑和1—异噁唑—2—异噁唑啉取代的-乙烯。

Fourthly, The preparation of 1 -triazolyl-2-isoxazolinyl substituted-ethenes was developed through an one-pot 1, 3-dipolar cycloaddition of NaN_3 and RI,α-alkylation reaction of substituted allyl bromides and 1, 3-dipolar cycloaddition of nitrile oxidesbased on polystyrene-supported propargyl selenide.

四、从聚苯乙烯负载的炔丙基硒醚出发,通过与叠氮化钠和碘化物的一锅法1,3-偶极环加成反应、取代烯丙基溴的α-烷基化反应和腈氧化物的1,3-偶极环加成反应固相合成了1—三唑—2—异噁唑啉取代的-乙烯。

In order to discuss the regioselectivity of nitrile oxide 1,3-dipolar cycloaddition to propyne , 1,3-dipolar cycloaddition reaction of substituted nitrile oxide (RCNO, R=F, NO2, OCH3, OH, COOCH3, CHO, CONH2, H, CH3) with propyne was studied using density functional theory at the 6-311++G** level, and the reaction rates were calculated at different temperature from 200 to 400 K.

用密度泛函B3LYP/6-311++G**方法研究了氧化腈(RCNO,R=F,NO2,OCH3,OH,COOCH3,CHO,CONH2,H,CH3)与丙炔的1,3-偶极环加成反应,并且计算了不同温度下的反应速率常数,讨论了氧化腈上不同取代基R的取代效应和温度对反应区域选择性的影响。

Selection of our products well, pure texture, the choice of materials are: acrylonitrile-butadiene rubber, silicone, ethylene-propylene rubber, fluoride plastic, hydrogenated nitrile, Poly-resin, folder cloth, rubber, PU expected, polytetrafluoroethylene, nylon, POM, engineering plastics (such as high-strength performance PPS, PEEK) and graphite (such as ordinary graphite, high - Pure graphite impregnated graphite), ceramics, alloys, Pan-gen, synthetic materials, etc.

我们的产品选材精良、质地纯正,选用的材料有:丁腈胶、硅胶、乙丙胶、氟胶、氢化丁腈、聚安脂、夹布、橡塑、PU料、聚四氟乙烯、尼龙、聚甲醛、工程塑料(如高强性能PPS、PEEK等);及石墨(如普通石墨、高纯石墨、浸渍石墨)、陶瓷、合金、盘根、合成材料等。

Selection of our products well, pure texture, the choice of materials are: acrylonitrile-butadiene rubber, silicone, ethylene-propylene rubber, fluoride plastic, hydrogenated nitrile, poly - Fat, folder cloth, rubber, PU expected, polytetrafluoroethylene, nylon, POM, engineering plastics (such as high-strength performance PPS, PEEK) and graphite (such as ordinary graphite, high-purity graphite impregnated Graphite), ceramics, alloys, Pan-gen, synthetic materials.

我们的产品选材精良、质地纯正,选用的材料有:丁腈胶、硅胶、乙丙胶、氟胶、氢化丁腈、聚安脂、夹布、橡塑、PU料、聚四氟乙烯、尼龙、聚甲醛、工程塑料(如高强性能PPS、PEEK等);及石墨(如普通石墨、高纯石墨、浸渍石墨)、陶瓷、合金、盘根、合成材料等。

In the first part, rhodium acetate catalyzed 1, 3-dipolar reactions of 1-diazo-2-oxo-propylphosphonates with nitriles was studied.

在催化量的醋酸铑作用下,1-重氮-2-羰基丙基膦酸酯与芳香腈顺利进行反应,而对脂肪腈的反应则很复杂,没有得到预期产物。

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