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The influence of each condition on the reaction speed and yield was studied, and the optimal conditions were: the ratio of the amount of substance of aromatic amine and heptafluoro-isopropyl iodine was 1:1.1~1.5, the amount of substance of sodium dithionite, sodium bicarbonate, aniline compounds were respectively 1.1~1.3, the amount of substance of phase transfer catalyst TBAB and aniline compounds was 0.05~0.1, the concentration of aniline compound was 0.5~1.0 mol/L, reaction temperature was 10~20 ℃, and the solvent was aether.

最佳结果为:芳胺与七氟异丙基碘的物质的量比1:1.1~1.5,连二亚硫酸钠、碳酸氢钠与苯胺的物质的量分别为1.1~1.3,相转移催化剂四丁基溴化铵与苯胺的物质的量比在0.05~0.1,溶剂总用量使苯胺浓度在0.5~1.0 mol/L;反应温度10~20℃;溶剂采用乙醚。取代基供电子性越强,反应时间越短,产率越高;氨基的对位优先反应,氨基的邻位较难发生反应;且七氟异丙基总是优先取代在芳环电子云密度较高的位置上。

In part one, the reactions of some active fluorine-containing compounds such as 2, 2-dihydropolyfluoroalkanoic acids and ethyl 2-hydropolyfluoroalkenoates were studied and various fluorine-containing heterocyclic compounds were synthesized. Using 2, 2-dihydropolyfluoroalkanoic acids as the starting material, 4-fluoroalkyl quinolin-2-ols, 2- [ -1-hydropolyfluoro-1-alkenyl] -4H-3, 1-benzoxazin-4-ones, 1-aryl -4, 9-dihydro-3-fluoro-alkyl-1H-pyrazo [3, 4-b] quinolin-4-ones, 5-fluoroalkyl-12H-quin olino [2, 1-b] quinazolin-12-ones, 4-fluoroalkyl-1, 3-dihydro-1, 5-benzodiazepin-2-ones and 4-fluoroalkyl-2H-pyrido [1, 2-a] pyrimidin-2-ones were synthesized through its condensation reaction with anilines, anthranilic acid, N'-aryl-o-aminobenzamides, o-nitro aniline, o-amino pyridine and their derivatives and the subsequent transformations. 5-Fluoroalkyl isoxazolidines, 3-fluoro-3-fluoroalkylisoxazolidino [4, 3-c] quinolin-4-ones, 3-fluoroalkylisoxazolino [4, 3-c] quinolin-4-ones and 2-aryl-3per fluoroacylindoles were synthesized by inter-and intramolecular 1, 3-dipolar cycloaddition of fluorine-containing olefins and nitrones.

第二部分,我们研究了α,α-二氟苄基卤类化合物的亚磺化脱卤反应、产物的转化及全氟烷基亚磺酸盐与芳环化合物的全氟烷基化反应,发现全氟苄基碘或溴及α,α一二氟苄基溴在保险粉等亚磺化脱卤试剂引发下可生成相应的亚磺酸盐;全氟苄基亚磺酸盐与氯气或溴反应可生成全氟苄基磺酰氯或磺酰溴;在烯烃存在下,全氟苄基碘则与烯烃发生加成反应,生成相应的1:1加成产物;在三价醋酸锰的作用下,部分芳香化合物如茴香醚,二甲氧基苯,吡啶,喹啉等可以和过量的全氟烷基亚磺酸盐发生双全氟烷基化反应,反应表现出一定的区域选择性,产率良好。

Bis-(4-bromobenzoyl) benzene as the monomer of poly was synthesized by Friedel-Crafts benzoylation reaction. Poly-Ⅱ synthesized via palladium-catalyzed aryl amination reaction using 1, 4-bis-(4-bromo-benzoyl) benzene and 4, 4'-diaminodiphenyl ether as monomers.

通过傅-克酰基化反应合成了1,4-双-(4'-溴苯酰基)苯,以1,4-双-(4'-溴苯酰基)苯和4'4-二氨基二苯醚为单体,通过钯催化的胺基化缩聚反应合成了高性能聚合物-聚亚胺酮-Ⅱ。

The invention discloses a dielectric hole-microhole composite material and synthesizing method in the inorganic porous material, adsorbing material and catalytic material technical domain, which comprises the following steps: adopting zeolite molecular sieve as raw material; reacting with sodium bisilicate solution under 30-60 deg.c for 10-300 min; disintegrating particle part of zeolite molecular sieve into piece with microhole structure; adding cetyl trimethyl ammonium bromide as molder; adjusting pH value of mother liquid to 10-12; aging 1-8h; adding in the high-pressure autoclave to do water heat synthesizing reaction at 80-130 deg.c for 24-72h; separating solid; washing; drying; sintering under 500-600 deg.c for 5-10h; obtaining the Si-Al porous material with dielectric hole and microhole composite structure.

本发明属于无机多孔材料、吸附材料和催化材料技术领域,涉及具有介孔-微孔复合材料及其合成方法。其特征是以沸石分子筛为原料,用偏硅酸钠的水溶液在30~60℃反应10~300分钟,使沸石分子筛的颗粒部分解离形成具有微孔结构的碎片,加入模板剂十六烷基三甲基溴化铵,然后调节母液pH值为10~12,老化1~8小时,然后加入高压釜于80~130℃进行水热合成反应。反应24~72小时后,分离出固体,水洗、干燥,然后于500~600℃焙烧5~10小时,得到具有介孔和微孔复合结构的硅铝多孔材料。本发明的效果和益处是所发明的合成方法可用于合成多种沸石结构和介孔结构的复合材料,所合成的材料经过质子交换可以具有较强的酸性,在吸附和催化领域具有广泛应用前景。

The effects of the surfactants, trioctyl phosphine oxide, sodium dodecyl sulfonate and hexadecyl trimethyl ammonium bromide, on the extraction rate of Co^2^+ were investigated. The acceleration in the kinetics in contributed to the associated molecule~2 TOPO taking part in the extraction process directly. The decrement effects of SDS or CTMAB on the rate of extraction kinetics of Co^2^+ with HDEHP were also observed, which caused by the adsorption of molecules of SDS or CTMAB on the interface and decreased the interfacial adsorption amount of HDEHP. In addition, the extraction rate was reduced by a bigger margin in HDEHP-SDS system. This can be explained in terms of the formation of an electric field at the interface.

研究体系中加入不同表面活性剂所引起萃取速率的不同改变:三辛基氧化膦因与HDEHP形成可萃取的Co^2^+活性分子缔合物,降低了萃取过程活化能而使反应加速;十二烷基磺酸钠和十六烷基三甲基溴化铵因占据发生萃取反应的界面区,减小了HDEHP与Co^2^+反应的机会而使反应减速; SDS还因其在界面形成较强的负电场,造成Co^2^+的附加势能而使萃取速率有更大幅度的降低。

The results of absorption spectra, KI fluorescence quenching studies, competitive binding studies and thermal denaturation experiments suggested that the interaction between AQS and DNA be intercalative.

在CT DNA存在下,KI对AQS光化学反应产物的荧光猝灭常数K〓比没有CT DNA存在情况下的要小。2.5×10〓mol/L的溴化乙锭即可将3.2×10〓mol/L的AQS从AQS与DNA的结合物中完全置换出来。

The phosphorus oxychloride or phosphorus tribromide N, N-dimethylformamide mix and react to form the Vilsmeier reagent used in the reaction. The newly prepared Vilsmeier reagent is added into the reaction bottle provided with the return condenser and the blender; a reaction raw material N, N-dimethylformamide solution expressed in the reaction formula is added into the system; the temperature is risen; the corresponding multi substituting pyridine-2 (1 H)-ketone compound can be made after the column chromatography of the silica gel; the production rate is between 60 and 95 percent according to different reactions.

由三氯氧磷或三溴化磷N,N-二甲基甲酰胺混合获得反应中所用Vilsmeier试剂;将新配制的Vilsmeier试剂加入装有回流冷凝管、搅拌器的反应瓶中,向体系中加入反应通式中表示的一种反应原料的N,N-二甲基甲酰胺溶液,升温,经硅胶柱层析分离得相应的多取代吡啶-2(1H)-酮类化合物,产率视不同反应在60~95%之间。

In this project, we have prepared conveniently Si-Mg 1,1-difunctional group reagents-α-silylvinyl Grignard reagents by hydromagnesiation of alkynylsilanes; Se-Br 1,1-difunctional group reagents-α-bromovinylselenides by hydrobromination of alkynylselenides; Sn-Br and Sn-I 1,1-difunctional group reagents by hydrozirconation of alkynylstannanes followed by halogenating reaction.

本项目通过炔基硅烷的镁氢化反应,方便地制得了Si-Mg 1,1-双官能团试剂-α-硅基烯基镁化物;通过炔基硒醚的溴氢化反应,方便地制得了Se-Br 1,1-双官能试剂-α-溴代烯基硒醚;通过炔基锡烷的锆氢化反应,继而卤代方便地制得了Sn-Br和Sn-I 1,1-双官能试剂。

The separation behavior of o hydroxybenzoic acid, m hydroxybenzoic acid and p hydroxybenzoic acid in high performance capillary zone electrophoresis was investigated using cetyltrimethylammonium bromide as reversed reagent for electroosmotic flow The effects of pH of buffer solution and volume fraction of methanol on the separation, peak shape and elution order were studie

采用十六烷基三甲基溴化铵为电渗流改性剂,考察了邻羟基苯甲酸、间羟基苯甲酸和对羟基苯甲酸在高效毛细管区带电泳模式下的分离行为,研究了缓冲液的pH和添加剂甲醇的用量对这 3种同分异构体的分离、峰形和出峰顺序的影响,并据此优化了这 3种异构体的分离条件。

The result shows that the elimination reaction and ring closing reaction are synergistic, and the hydrogen in the elimination reaction derives from hydroxyl. In addition, the activation energy of the reaction is 139.2kJ/mol.

计算结果表明,该反应中的消除反应和成环反应是协同进行的,溴化氢消除反应中的氢来自与O(22)相连的羟基氢,反应的活化势垒为139.2kJ/mol,反应放热25.1kJ/mol。

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