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酰化

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At last,a convergent and general protocol to marine natural product,as demonstrated by the enantioselective total synthesis of malyngamides O,P,Q,R, 5"-epi-Q and 5"-epi-R bearing terminal vinylic chloride structure,was developed in detail.E,(7S)-7-methoxytetradec-4-enoic acid was prepared using the above described Johnson-Clainsen rearrangement,the terminal vinyl chloride was constructed using Wittig reaction as key step,the pyrrolidone derivative was constructed using L-serine as natural chiral pool.Starting from the synthesis of malyngamides O and P to explore the general route,an aldol reaction of methyl acetate with the vinyl chloride part in the presence of LDA gave the skeleton of amine portion,followed by amidation with the fatty acid finished the synthesis of malyngamide P.

先以malyngamides O和P为试点探索通用合成路线,将乙酸甲酯和烯氯部分在LDA存在下进行aldol反应得到氨部分的骨架,再将手性不饱和脂肪酸和氨部分进行酰胺化反应完成了malyngamide P的合成,将P在碱性条件下进行烯醇甲基化反应完成了malyngamide O的全合成。

Research result indicated that the cooperative effect between swell and precursor is main factor for the nanoparticle loaded in Nafion, and moreover, polarity of solvent and water content in Nafion also affects the load largely. To improve away the surface concentration of CdS nanocrystal on two side of membrane for general preparation, thioacetamide was first used as a precursor instead of inorganic sulfur source(H2S and Na2S) in synthesis of CdS nanocrystal. The assembly mechanism for several sulfur source had been studied, and CdS/Nafion with the character of homogeneous disperse had been prepared, which is fit for mass transmission in photocatalitic reaction. Following the investigation of several crystallizing way, simple and reliable hydrothermal-crystallizing was found. According to this way, maximal TiO2 load in Nafion achieved 43%. Activity of TiO2/Nafion or CdS/Nafion as a photocatalyst was explored initially for disintegrating liquid contamination. Maximal decompose rate achieved 86% under condition of this research.

研究结果表明:Nafion膜对纳米粒子负载量的主要影响因素是溶胀作用与前驱体协同效应,同时溶剂极性和薄膜含水量对负载量也影响相当大;本课题首次使用硫代乙酰胺代替传统无机硫源(H2S、Na2S)合成CdS纳晶,研究了各种硫源的组装机理,克服了常规技术存在的CdS纳晶趋于膜表面富集的缺点,得到了有利于光催化传质需要的体相均匀分布CdS/Nafion;研究了多种Nafion膜内纳米粒子晶化途径,找到了简单可靠的水热晶化法,TiO2纳晶最高负载量达43%;初步探索了TiO2/Nafion、CdS/Nafion作为光催化剂降解水中模拟污染物的活性,在本实验条件下最高降解率达86%。

The method was validated for acetylated peptides and allowed an assessment of even the basal protein phosphorylation of phenylalanine hydroxylase in intact cells.

该方法被确证乙酰酶多肽,并允许在不完整细胞中对苯丙氨酸羟化酶的基本蛋白质磷酸化的评估。

Firstly, the 10-methoxy-5H-dibenzazepine is synthesized through brominating and methoxylation and hydrolyzation from 5H-dibenzb, fJazepine-5-carbonyl chloride.

首先,研究了以5-氯甲酰基亚氨基芪为原料,经溴化、甲氧基化、水解合成了10-甲氧基亚氨基芪。

Four substances including 2-methyl ethyl acetoacetate and barley straw extract distilled from bulrush as well as cetyl trimethyl ammonium bromide and isothiazo lintone were used for the comparison experiment in inhibiting the growth of Microcystis aeruginosa in various phases. Result showed that inputting chemicals in the lag phase has better effect than in the log phase, and adding in lag phase can effectively inhibit the algae growth. Although feeding allelopathic substance at log phase can lead to certain restraining effect, it cannot result in the effective inhibition of algae growth, which can be well achieved by feeding CTAB and isothiazo lintone below 10mgl/L during log phase.

研究用从芦苇中提取的2-甲基乙酰乙酸乙酯和大麦秸浸出液两种化感物质以及十六烷基溴化钱和异噻唑啉酮等四种药剂对不同生长期的铜绿微囊藻进行了对比抑制试验,结果显示在铜绿微囊藻生长的迟缓期投加试验药剂效果比在对数期投加效果都好,在迟缓期投加四种药剂,都有很好的抑藻效果;在铜绿微囊藻生长的对数期投加化感物质,虽然有一定的抑藻率,但效果较差,而在藻对数期投加10mg/L以下的CTAB和异噻唑啉酮能达到很好的水华抑制效果。

However, no examples of a copper-catalyzed combination of N-alkenylation and N-alkylation of amides had been reported.

然而,组合铜催化的酰胺N—烯基化和N—烷基化偶联生成二氢吡咯衍生物的反应未见文献报道。

It was shown that the absorption peaks of amine and amide groups of gelatin were shifted in HDPE/PE-g-MAH/Gelatin blends because of the reaction of PE-g-MAH with gelatin. The addition of PE-g-MAH made the increase of HDPE glass transition temperature. The compatibilizing effect of PE-g-MAH was due to the crystal compatibility produced by forming the co-crystals of HDPE, PE-g-MAH and PE-g-MAH-g-gelatin. The blends of EAA and gelatin were prepared by melting process and the compatibility of the blends was also studied.

红外光谱分析结果表明:体系中明胶的氨基吸收峰、酰胺Ⅱ带吸收峰峰位发生了明显的变化;二甲苯和水抽提实验表明,在熔融共混过程中EAA与明胶发生了反应;DMA测试共混物的玻璃化转变温度发现:两组分的玻璃化转变温度差值减小;SEM的实验结果表明,共混物中明胶的表面有接枝物形成。

The blends of PE-g-MAH and gelatin were prepared by melting process and the compatibility of PE-g-MAH and gelatin in blends were characterized. The results of FTIR showed that the characteristic absorption band peaks of amine and amide groups of gelatin were shifted in PE-g-MAH/Gelatin blends, the equilibrium values of torque were higher with the increase of blending temperature, which proved that graft copolymer PE-g-MAH-g-gelatin was formed during the preparation process, and the amount of PE-g-MAH-g-gelatin was increased with increasing the amount of PE-g-MAH. SEM micrographs exhibited that there was PE-g-MAH-g-gelatin formed in surface of gelatin phase.

通过红外光谱分析、HAAKE流变分析、抽提等实验证明:共混物中明胶的氨基、酰胺基团吸收峰峰位发生了明显的变化;在熔融共混过程中,随着温度的提高,平衡扭矩增大;明胶与PE-g-MAH发生了反应形成PE-g-MAH-g-明胶接枝共聚物,而且随着PE-g-MAH用量的增加,形成接枝共聚物的量也提高;SEM的实验结果表明,在明胶的表面确有接枝物形成;通过DMA测试共混物的玻璃化转变温度,发现两组分的玻璃化转变温度差值减小,二者的相容性提高,实现了共混体系的自增容。

It was shown that the absorption peaks of amine and amide groups of gelatin were shifted in HDPE/PE-g-MAH/Gelatin blends because of the reaction of PE-g-MAH with gelatin. The addition of PE-g-MAH made the increase of HDPE glass transition temperature. The compatibilizing effect of PE-g-MAH was due to the crystal compatibility produced by forming the co-crystals of HDPE, PE-g-MAH and PE-g-MAH-g-gelatin. The blends of EAA and gelatin were prepared by melting process and the compatibility of the blends was also studied. The FTIR results showed that absorption peaks of amine and amide groups of gelatin were shifted in EAA/Gelatin blends.

通过红外光谱分析、HAAKE流变分析、抽提等实验证明:共混物中明胶的氨基、酰胺基团吸收峰峰位发生了明显的变化;在熔融共混过程中,随着温度的提高,平衡扭矩增大;明胶与PE-g-MAH发生了反应形成PE-g-MAH-g-明胶接枝共聚物,而且随着PE-g-MAH用量的增加,形成接枝共聚物的量也提高;SEM的实验结果表明,在明胶的表面确有接枝物形成;通过DMA测试共混物的玻璃化转变温度,发现两组分的玻璃化转变温度差值减小,二者的相容性提高,实现了共混体系的自增容。

The main work of the article was to synthesize a suitable monomer, bis(4-carboxyphenyl)phenyl phosphine oxide, as the retardant for poly fibre. The procedures were divided into three steps: dichloride phenyl phosphine oxide was synthesized and bis(4-methyl phenyl)phosphate oxide was prepared from DCPP by Friedel-Crafts reaction.

双苯基氧化膦是一种适用于PET纤维阻燃改性的新型有机磷阻燃剂,本文主要研究了其合成工艺,整个合成路线分为三步,通过Friedel-Crafts烷基化反应制备了苯基二氯化膦,进而通过Friedel-Crafts酰基化反应合成了双苯基氧化瞵,经氧气、高锰酸钾氧化得到了产品BCPPO。

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