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The optimum conditions were reaction temperature 120°C, reaction time 20h, mole ratio of 5-chloromethyl-2-oxazolidinone and sodium phenolate 1:1. 3,5-Dimethylphenol and epichlorohydrin in sodium hydroxide were condensated to give l,2-epoxy-3-phenoxy propane, then the reation of l,2-epoxy-3-phenoxypropane and the carbamate afforded oxazolidinone in the yields of 69.0%~76.0%. The side reaction had been avoided effectively by the uses of the excessive epichlorohydrin and mixed catalysts.

用3,5-二甲基苯酚和环氧氯丙烷在氢氧化钠存在下缩合生成苯氧基环氧丙烷,然后和氨基甲酸酯反应生成噁唑烷酮,采用过量环氧氯丙烷和使用混合催化剂,有效的避免了副反应的发生,提高了噁唑烷酮的产率,产率69.0%~76.0%。

In this thesis, we did modifications of alkyl groups upon benzyl fluorophosphonate. In order to study the influence of alkyl length and steric effect on activity and selectivity of probes, we synthesized benzyl fluorophosphonate recognition heads with modifications including ethyl, butyl, octyl and cyclohexyl. By way of connecting different kinds of tag like azido group, biotin and rhodamine with recognition heads separately through a higher hydrophilic ethylene glycol derived linker, a series of benzyl fluorophosphonate probes were made up. And they will apply to various biological testing strategies.

在本论文中,我们以苯甲基氟化磷酸酯为基础,於其上进行一系列烷基之修饰,为了探讨烷基长度与空间立体性质对於探针活性及选择性的影响,我们合成了包含乙烷基、丁烷基、辛烷基以及环己烷基修饰的苯甲基氟化磷酸酯辨识端,并藉由具较高亲水性的聚乙二醇衍生连接桥结合三种不同的发报端,分别有叠氮基团、生物素及萤光基团来构成不同的化学探针组合,这一系列苯甲基氟化磷酸酯类化学探针将可被应用於不同的生物测试策略。

The cure reactions of ternarysystem containing poly, poly and HDI isocyanurate, and the effect of the ratio ofPGA/POH on the thermal, mechanical and surface properties of curedresin have also been examined.

本文还研究了聚丙烯酸环氧丙酯、聚丙烯酸羟丙酯和六亚甲基二异氰酸酯三聚体的反应及三元反应体系中PGA/POH的不同比例对交联后树脂的热性能、力学性能及表面性能的影响。

The aim of this study was to develop a novel amphiphilic functional block poly(ε-caprolactone) bearing ketone groups MPEG-b-P(OPD-co-CL. 2-oxepane-1, 5-dione was copolymerized with ε-caprolatone in which methoxy poly (MPEG, Mn=5 000) and stannous octoate were used as initiator and catalyst, respectively. The syntheses were conducted by bulk and solution polymerization. 1H NMR results showed that peak position and splitting of the polymers synthesized through solution polymerization were consistent with theoretical data, demonstrating the products were designed block copolymers. While in the bulk polymerization, polymer peak position was changed due to their high reaction temperature, suggesting their structural variation.

将带有羰基官能团的4-羰基己内酯和ε-己内酯分别在甲氧基聚乙二醇(MPEG,Mn=5 000)为引发剂,异辛酸亚锡为催化剂溶液和本体体系中开环聚合,合成了两亲性侧基带有羰基官能团的聚己内酯嵌段共聚物MPEG-b-P(OPD-co-CL.1H NMR结果表明采用溶液聚合法合成的聚合物各峰的峰位置和分裂情况与理论一致,证明了产物是实验所设计的嵌段共聚物,而采用本体聚合法合成的聚合物由于温度的影响,聚合物各峰的峰位置发生了变化,说明其结构发生了变化;差示扫描量热法分析结果表明随着OPD单体含量的增加,聚合物的熔点,玻璃化转变温度和熔融焓增加;热失重测试结果表明OPD单体的引入增加了聚合物的热敏感性。

Mono(2-hydroxy propyl)phosphate was synthesized from 1, 2-epoxy propane and phosphoric acid in the propanone solvent under the conditions of reaction temperature 30 ℃, reaction time 2 h.

摘 要:以环氧丙烷、磷酸为原料合成了磷酸单( 2-羟基丙基)酯,并以磷酸单(2-羟基丙基)酯和三氧化二锑为原料合成了磷酸单(2-羟基丙基)酯锑。

In this paper, 4-4-(trifluoromethoxy benzoyl cyclohexyl-3, 5-diaminobenzoate with a large branch chain, pyromellitic dianhydride and 4-(4-aminobenzyl) benzenamine were used to synthesize polyimides. The effect of monomer charge order on pretilt angle was investigated for the first time when PIs were used as LC alignment layer, and the effect of diamine mole ratio on pretilt angle was studied. The thermal stability of the pretilt angle was discussed.

文章用均苯四酸二酐、4,4'-二胺基二苯甲烷和具有较大支链的4-(4-苯甲酰基)环己基-3,5-二胺基苯甲酸酯等单体制备聚酰亚胺,首次研究了单体加料顺序对液晶预倾角的影响,同时也研究了二胺配比对液晶预倾角的影响问题,并探讨了预倾角的热稳定性等问题。

Methods 4-Hydroxy- benzonitrile was treated with sodium hydrogen sulfide and anhydrous magnesium chloride in dimethyl formamide to give thioamide, which was then directly cyclized with ethyl 2-chloroacetoacetate without separation to give ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(2) in one-pot; then 2 was formylated with Duff reaction adopting hexamethylenetetramine in trifluoroacetic acid to give ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(3); finally, the target compound was obtained by the treatment of 3 with hydroxylamine hydrochloride and sodium formate in formic acid.

采用&一勺烩&方法,以4-羟基苯甲腈为起始原料,首先与硫氢化钠和无水氯化镁在N,N-二甲基甲酰胺中反应,所得中间体不经分离,直接加入2-氯乙酰乙酸乙酯进行环合反应,得到2-(4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(2);然后通过六亚甲基四胺/三氟乙酸进行Duff反应,得到2-(3-甲酰基-4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(3);再经盐酸羟胺/甲酸/甲酸钠体系脱水得到目标化合物。

In this dissertation, preparation of polysubstituted ethene and heterocyclic compounds based on 2-hydroxyalkyl phenyl selenides andα-phenylselenopropionic acid reagents were further investigated as follow: Firstly, O-ethyl-O-vinyl phosphonates were prepared in a one-pot, two-step transformation by Mitsunobu reaction of 2-hydroxyalkyl phenyl selenides with monoethyl esters of phosphonic acid in the presence of diethyl azodicarboxylate and triphenyl phosphine (PPh3) followed by oxidation-eliminatio...

中文摘要:本文主要进一步探索了2-羟基烷基苯基硒醚、α-苯硒基丙酸试剂在制备多取代乙烯和杂环化合物反应中的应用,具体研究内容和结果如下:一、在偶氮二羧酸乙酯和三苯膦(PPh3)存在下,苯基-2-羟基烷基硒醚和O-乙基膦酸单酯发生Mitsunobu反应,无需分离和纯化反应中间体,直接使用30 %的双氧水进行氧化-消除反应,提供了&两步、一锅&合成O-乙基-O-乙烯基膦酸酯的新方法,该方法反应条件温和,操作简便,产物收率良好(76-82 %)。

In the mixed solvent of dimethyl phthalate / TBP or phenyl ether / TBP, the selectivity for styrene oxide is good but the conversion of styrene is low due to the coordination to the catalyst of the solvent.

邻苯二甲酸二甲酯或二苯醚等与磷酸三丁酯的混合溶剂中环氧化的选择性较高,但由于溶剂对催化剂的配位作用抑制了催化剂的活性,苯乙烯转化率很低;当部分的邻苯二甲酸二甲酯或二苯醚被甲苯取代后,苯乙烯的转化率提高,生成环氧苯乙烷的选择性不变。

In this thesis, this system is used for epoxidation of propylene and styrenewith good results. The solvent effect is investigated for epoxidation of styrene. In the mixedsolvent of dimethyl phthalate / TBP or phenyl ether / TBP, the selectivity for styreneoxide is good but the conversion of styrene is low due to the coordination to thecatalyst of the solvent. When part of dimethyl phthalate or phenyl ether is replacedby toluene, the conversion increases and the selectivity keeps constant.

邻苯二甲酸二甲酯或二苯醚等与磷酸三丁酯的混合溶剂中环氧化的选择性较高,但由于溶剂对催化剂的配位作用抑制了催化剂的活性,苯乙烯转化率很低;当部分的邻苯二甲酸二甲酯或二苯醚被甲苯取代后,苯乙烯的转化率提高,生成环氧苯乙烷的选择性不变。

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