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乙酰胺

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Preparation of ethylene bis stearamide using stearyl chloride and ethylenediamine as raw materials has been studied.

研究了以乙二胺和硬脂酰氯为原料制备乙撑双硬脂酰胺的反应,讨论了原料配比、反应时间、反应温度的影响。

The reaction of benzoic acid and ethylenediamine was studied under different conditions.

在不同条件下考察了苯甲酸与乙二胺的反应,对反应产物、主要副产物及反应中间体进行了分离和鉴定,通过熔点测定、元素分析和红外光谱分析,确定了产物为2-苯基咪唑啉,主要副产物为二苯甲酰乙二胺,中间体之一为乙二胺与苯甲酸形成的双盐。

In this study the incidence of acute mountain sickness was 24% for people taking 125 mg twice daily, 21% for people taking 325 mg twice daily, and 51% for people taking placebo.9

在这项研究中,急性高空病的发病率在应用乙酰唑胺125mg2次/天组为24%,在应用乙酰唑胺325mg2次/天组为21%,在应用安慰剂组为51%[9]。

A series of p-toluene sulfonylamido acetacylhydrazone derivatives were synthesized from p-toluenesulfonyl chloride which reacted with glycine to get the intermediate p-toluene sulfonylamido glycine, then through the esterification, hydrazinolysis to afford another intermediate p-toluene sulfonylamido acethydrazide, which condensed with different aldehydes to obtain the target compounds that were characterized by IR, 1H NMR, 13C NMR spectra and elemental analysis.

魏太保 ;冷艳丽;王永成;张建辉;张有明*摘要:以对甲苯磺酰氯为原料,通过与氨基乙酸反应得到中间体对甲苯磺酰氨基乙酸,再经酯化、肼解得到对甲苯磺酰氨基乙酰肼,然后与相应的醛缩合得一系列对甲苯磺酰胺基乙酰腙类化合物。其结构经元素分析, IR, 1H NMR和13C NMR确证。

In this thesis,the AM1,MNDO,MINDO/3(mainly AM1)and INDO/S-CI semiempirical MO methods were used toinvestigate the excited-state intramolecular protontransfer reactions of salicylic acid derivatives—salicylic acid,methyl salicylate,salicylaldehyde,o-hydroxyaceto-phenone,salicylamide and 3-hydroxy-picolinamide (6 conformers and 2-3 anion species);2-(2'-hydroxy-5' methylphenyl) benzotriazole(4 conformers),2-(2' hydroxyphenyl) benzimidazole (3 conformers and 3anion species),Bis-2,5-(2-benzoxazolyl)hydroquinone(3 conformers),2-(2'-hydroxyphenyl)benzothiazole(2conformers) and 7-azaindole dimer (2 conformers).Theinvestigations were described as follows.Geometry optimization,relative stability andhydrogen bonding energy First,for sylicylic acid derivative molecules,the AM1,MNDO and MINDO/3 methods were used toinvestigate ground-state geometry optimization,energies,relative stabilities and hydrogen-bondingenergies on the five kinds of the molecules(designing 6 conformers and 2-3 anion species).Comparing with experimental data,the optimizedgeometry,the order of stability,the hydrogen-bonding energies and the distances between O-O in O-H..O hydrogen bonds by AM1 method were in agreementwith the experimental data,however,the C-C bondlengths optimized by MNDO and MINDO/3 were longer,C-O and O-H bond lengths were shorter;for C-N bondlengths,the results opitimized by MNDO method werethe same as those by AM1 method,nevertheless the C-Nbond lengths given by MINDO/3 method were muchshorter.For some sylicylic acid derivatives(e.g.methyl salicylate,salicylamide),the order ofstabilities on the conformers given by MNDO andMINDO/3 methods were not in agreement with theexisting conformers deduced by experimental methods,and the hydrogen bonding energies calculated by MNDO.and MINDO/3 methods were smaller.Second,the studyon the other systems found that the optimizedgeometry of the proton-transfered product with INDOmethod could not be obtained,only could theoptimized geometry of reactant be obtained,and thecalculated hydrogen bonding energies were greater.Many results of calculation indicated that the studyon the excited-state intramolecular proton transferreaction system using AM1 method was suitable andreliable.

本论文用AM1、MNDO、MINDO/3(主要是AM1)和INDO/S-CI半经验分子轨道方法对水杨酸衍生物系列——水杨酸、水杨酸甲酯、水杨醛、O-羟基乙酰苯酮、水杨酰胺和3-羟基吡啶酰胺(6种异构体和2-3种阴离子);2-(2'-羟基-5'-甲基苯基)苯并三〓唑(4种异构体);2-(2'-羟基苯基)苯并咪唑(3种异构体和3种阴离子);2,5-二间氮杂氧茚氢醌(3种异构体);2-(2'-羟基苯基)间〓杂硫茚(2种异构体)和7-〓吲哚二体(2种异构体)的激发态分子内质子转移反应在以下几个方面进行了较系统的理论研究:几何构型优化和相对稳定性及氢键能首先以水杨酸衍生物系列分子为例,用AM1、MNDO和MINDO/3方法考察了5种分子(每种分子设计6种异构体和2-3种阴离子)的基态几何构型优化,能量、相对稳定性和氢键能计算,通过和实验数据进行比较,AM1方法给出的优化几何构型、稳定性次序、氢键能和O—H。。。O氢键的0—0距离与实验数据吻合最好,MNDO和MINDO/3方法优化的C-C键长偏长,C-O键和O-H键长偏短;对于C-N键长,MNDO和AM1优化结果差别不大,而MINDO/3给出了过短的C-N键长,MNDO和MINDO/3方法给出的有些水杨酸衍生物分子(如水杨酸甲酯和水杨酰胺)异构体的稳定性次序和实验上推测的可存在异构体结果不一致,MNDO和MINDO/3方法给出的氢键能偏低,对其他体系的研究发现INDO方法常常不能得到质子转移产物的优化几何构型,只能得到反应物的优化构型,并且估算的氢键能偏高,大量的计算结果表明AM1方法对本论文研究的激发态分子内质子转移反应体系是适宜和可靠的。

Synthesis process of 2,6-dichloro-3-methylaniline was investigated 3-methylaniline was first N-acetylated with acetic anhydride,then treated with chlorosulphonic acid and ammonia yielding the 2-methyl-4--benzenesulfonic amide,which wasin turn deacetylated,chlorinated and hydrolyzed to the title compound.Hydrochloric acid was used instead of sodium hydroxide in deacetylation and sodium chlorate instead of hydrogen peroxide as oxidant in chlorination.

合成工艺2,6-二氯-3-甲基苯胺调查3-甲基首次N-乙酰与醋酸酐,然后与氯磺酸和氨产量 2-甲基-4--苯磺酰胺基,而擅转乙酰,氯化和水解的标题compound.hydrochloric酸代替氢氧化钠乙酰氯酸钠代替双氧水为氧化剂,加氯。

Synthesis of Antidote of N-Dichloroacetyl-2-methyl-1-oxa-4-aza-spiro-4.4-nonane BI Hong-mei, ZHANG Jin-yan, LIANG Ying, SHEN Yong (College of Arts and Sciences Heilongjiang August First Reclamation University, Daqing 163319, Heilongjiang, China) Abstract: N-Dichloroacetyl-2-methyl-1-oxa-4-aza-spiro-4.4-nonane was synthesized by one pot method with isopropanolamine, cyclopentanone and dichloroacetyl chloride. The optimum reaction conditions obtained are as follows:the proportion in moles of the above materials is 1∶1∶1.2, reaction solvent is toluene, reaction temperature is -15 to -10 ℃,reaction time is 3 h, under the optimum condition, the yield of the compound is 50.0%.

除草剂解毒剂N-二氯乙酰基-2-甲基-1-氧杂-4-氮杂-螺[4.4]壬烷的合成毕洪梅,张金艳,梁英,沈勇(黑龙江八一农垦大学文理学院,黑龙江大庆 163319)摘要:以33%的氢氧化钠水溶液为缚酸剂,异丙醇胺、环戊酮和二氯乙酰氯为原料,采用&一锅法&合成了N-二氯乙酰基-2-甲基-1-氧杂-4-氮杂-螺[4.4]壬烷,采用正交实验法得到最佳反应条件:反应原料摩尔比为1∶1∶1.2,苯作溶剂,反应的温度为-15 ℃~-10 ℃,搅拌时间为3 h,产率达到50.0%。

A process for preparingp-fluo-2-(2-methyl-3-propionyl)-4-oxy-N,3-diphenyl-phenylbutylamide includes such steps as Friedle-Craft acylating of newly prepared phenylacetyl chloride and fluorobenzene under catalysis of AlCl3 to obtain 4-fluoro-phenylbenzyl ketone, brominating at carbonyl alpha position under catalysis of less AlCl3 to obtain alpha-bromo-4-fluo-phenylbenzyl ketone, and condensing with isobutyryl acetanilide under action of sodium ethoxide.

本发明涉及一种制备对氟-2-(2-甲基-3-氧丙基)-4-氧-N,3-二苯基-苯丁酰胺(1)的方法,其包括以下步骤:新制的苯乙酰氯与氟苯在AlCl3催化下进行Friedle-Craft酰化反应,得到对4-氟-苯基苄基酮(4);化合物(4)在少量AlCl3催化下进行羰基α位溴化,得到α-溴-4-氟-苯基苄基酮(5);然后(3)异丁酰乙酰苯胺在乙醇钠作用下与化合物(5)进行缩合。

Hydrophobic-hydrophilic macroporous polydivinylbenzene/polyacrylethylenediamine interpenetrating polymer networks (PDVB/PAEM IPN) were prepared by the sequential suspension polymerization method. These were composed of two networks, of which one was hydrophobic and the other was hydrophilic. The objective of this work was to study the adsorption thermodynamics and adsorption kinetics of this hydrophobic- hydrophilic IPN. The focus was on adsorption isotherms of vanillin at different temperatures, and these fit well into the Freundlich adsorption isotherm. The isosteric adsorption enthalpy, adsorption Gibbs free energies and the adsorption entropy could be calculated according to thermodynamic functions.

采用分步悬浮聚合法制备了具有疏水性能的聚二乙烯基苯(polydivinylbenzene, PDVB)为第一网,具有亲水性能的聚丙烯酰乙二胺(polyacrylethylenediamine, PAEM)为第二网的疏水/亲水大孔聚二乙烯基苯/聚丙烯酰乙二胺互穿聚合物网络(interpenetrating polymer networks, IPN),研究这类疏水/亲水IPN组成的树脂对吸附质的吸附热力学和吸附动力学;测定了该树脂对香兰素在不同温度下的吸附等温线,吸附等温线符合Freundlich等温吸附方程,利用热力学函数关系计算出了吸附焓、自由能和熵变。

The resultedα-methylamine was protected by acetyl chloride, and then was chlorosulfonated bychlorosulforic acid at -5℃-0℃followed by treatment with aqueous ammonia givingcompound A in 52.3% yield.

甲基胺再用乙酰基进行保护后,以HSO3Cl为试剂进行氯磺化反应,再用浓氨水进行反应,制得了乙酰基保护的苯磺酰胺类化合物。

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