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Part 2. Annulation reaction of 3, 4-dichlorocoumarin (1) and 3, 4-dichloromaleimide (8) by a new general annulation strategy developed in this group with 2-phenylbenzofuran (15), 3-phenylbenzofuran (16), 2, 5-diphenyloxazole (17), 2, 5-diphenylthiazole (18), 2-methyl-4-phenylthiazole (19) and 2, 3-dimethoxy-1, 3-butadiene (40) were investigated.

二。在本课题组前一阶段提出的从二氯代环烯酮与1,1-二芳基乙烯的光化反应以及光化反应中得到的环丁烷产物的连续电环化反应对3,4-二氯马来酰亚胺以及3,4-二氯香豆素进行增环反应的工作基础上,研究了3,4-二氯香豆素(1)和3,4-二氯马来酰亚胺(8)与5个α-苯基取代的环烯烃2-苯基苯并呋喃(15),3-苯基苯并呋喃(16),2,5-二苯基噁唑(17),2,5-二苯基噻唑(18),2-甲基-4-苯基噻唑(19),以及一个丁二烯——2,3-二甲氧基丁二烯(40)进行的芳香族增环反应。

In our research on study chemical reaction of active methylene compounds and brom-acetophenone. Because of brom-acetophenone is compound that contain carbonyl and halogen ,which will take place electrophilic substitution and nucleophilic addition. When active methylene compounds are ethyl acetoacetate and β-diketone, controlling reaction condition, we have found that mono-substitution's production and di-substitution's. production is isolated; active methylene compounds are acetoacetanilide and acetoacetanilide derivate, pyrrolidin-2-one derivants were obtained by substitution and close-ring reaction .but there is no report about it.

本文是让活泼亚甲基类化合物与溴代苯乙酮发生化学反应,由于溴代苯乙酮是含有羰基的卤代烃结构,它可以发生亲电取代和亲核加成反应,当活泼亚甲基类化合物为乙酰乙酸乙酯和β-二酮时,控制反应条件可以发生单取代和双取代两种产物;当活泼亚甲基类化合物为乙酰乙酰芳胺类化合物来反应时,溴代苯乙酮中的羰基与氨基会发生分子内的关环反应生成吡咯烷-2-酮衍生物,这在以前的研究中是没有发现的。

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。

Amino-monomethoxypoly(ethy1ene glycol)(mPEG-NH2) was synthesized based on the principle of Gabriel synthesis.Monomethoxypoly(ethy1ene glycol) tosylate was prepared at first,and then reaction with potassium salt of phthalimide as nucleophile to produce the monomethoxypoly(ethy1ene glycol)phthalimide derivative.

摘 要:首先合成了单甲氧基聚乙二醇对甲苯磺酸酯,然后根据盖布瑞尔合成法原理,以邻苯二甲酰亚胺钾盐为亲核试剂与mPEG-OTs反应,生成单甲氧基聚乙二醇的邻苯二甲酰亚胺衍生物,mPEG-PI与水合肼反应肼解生成伯胺,合成了一端为氨基的单甲氧基聚乙二醇(mPEG-NH2)。

Gabriel reaction was adopted to synthesis 2-(0ctahydro-1-azocinyl)ethylamine, N-(β-Heptamethyleniminoethy1)phthalimide was prepared by treating Heptamethylenimine with N -(β-bromoethy1) phthalimide. N -(β-bromoethy1) phthalimide was easily prepared from phthalic anhydride in two steps.

我们采用Gabriel伯胺合成法制备2-环庚亚胺基乙胺,从邻苯二甲酸酐经过两步反应很容易地得到N-邻苯二甲酰亚胺,然后与环庚亚胺发生亲核取代反应,产物再水解制得伯胺2-环庚亚胺基乙胺。

Two new active esters of acrylic acids monomers, N-p-acryloxybenzoyloxy succini-mide and N-p-methacryloxybenzoyloxy succinimide have been synthesized and polymerized.ABOSu and MBOSu were prepared by coupling of p-acryloxybenzoic acid or p-methacryloxybenzoie acid with N-hydroxy succinimide in the presence of dicyclohexylcarbodimide.

新的丙烯酸活性酯,N-(对甲基丙烯酰氧苯甲酰氧基)丁二酰亚胺及N-丁二酰亚胺单体分别由对甲基丙烯酰氧基苯甲酸、对丙烯酰氧基苯甲酸与N-羟基丁二酰亚胺在环已基羰二亚胺存在下经偶联反应合成。

A convenient method to synthesize three kinds of novel 2-(2-hydroxyphenyl) benzimidazole in order to improve the solubilities of the fluorophores with substituent of carboxyl, ester and double-bond which are aimed for determining the sulphydryl group was reported.

合成了N-{3-(2-苯并咪唑基)-4-羟基苯基}马来酰亚胺酸, N-{3-(2-苯并咪唑基)-4-乙酸酯基苯基}和马来酰亚胺N-{3-(2-苯并咪唑基)-4-羟基苯基}马来酰亚胺,在基本荧光发射团上分别引入了羧酸基;酯基;双键活性基团。

Benzoyl chloride was treated with potassium selenocyanate in dichioromethane by using polyethylene glycal-400 as the solid-liquid phase transfer catalyst to yield the corresponding benzoyl isoselenocyanate. This intermediate did not need to be isolated and directly reacted with arylamines, affording the N-benzoyl-N'-arylselenoureas 2a~2p. These compounds were characterized by IR, 1H NMR spectra and elemental analysis and the single crystal structure of 2k has been confirmed by X-ray crystallographic analysis.

以PEG-400为固液相转移催化剂,通过苯甲酰氯与硒氰酸钾反应合成了中间体苯甲酰基异硒氰酸酯,该中间体不需分离,直接与芳胺反应,得到N-苯甲酰基-N'-芳基硒脲(2a~2p),这些化合物用1H NMR,IR及元素分析进行了表徵,并用X射线单晶衍射确定了化合物2k的单晶结构。

The UHF/AMl calculations were applied to study the thermolyses of o- dimethylaminobenzoyl, o-dimethylamino-p-methylbenzoyl and o- dimethylamino-p-nitrobenzoyl azides.

采用UHF/AM1方法对2-二胺基苯甲酰叠氮、2-二甲胺基-3-甲基苯甲酰叠氮和2-二甲胺基-3-硝基苯甲酰叠氮的热分解反应进行了研究。

Firstly, phenyliodine diacetate was immobilized to the 2% cross-linked polystyrene or the liner polystyrene resin. The more iodine the resin had, the lower conversion to phenyliodine diacetate. We made our endeavor to extend the range of useful application of polystyrene supported phenyliodine diacetate in organic synthesis:(1) the reagent was used as an effective reagent of carbonyl regeneration from oximes and semicarbazones of ketones.(2) the reagent was also applied to the synthesis of 1, 3, 4-oxadiazoles, 1, 3-disubstituted-2-pyrazoline, 2-arylbenzoxazole from aldehyde N-acylhydrazones, aldehyde hydoazones and phenolic Schiff's bases respectively.

首先,我们以2%交联的聚苯乙烯和线性的聚苯乙烯树脂为载体,制备了聚合物负载的二醋酸碘苯,通过研究发现:(1)聚苯乙烯二醋酸碘苯是酮肟、缩氨脲有效的去保护试剂,不仅芳香酮,脂肪酮和α,β不饱和酮的肟、缩氨脲也能顺利转化为相应的酮,实现酮基的再生;(2)我们还利用此试剂,分别与醛的N-酰基苯、N-酰基苯腙及邻羟基芳亚胺反应,在温和的条件下发生成环反应,以良好的产率生成1,3,4-噁二唑、吡唑啉和二取代苯并噁唑等杂环化合物;(3)聚苯乙烯二醋酸碘苯还可有效地将邻羟基芳酮的酰腙经氧化、重排成1,2-二酰基苯。

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