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苯甲腈

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We provide intermediates of Methylphenidate HCl: 2-Phenyl-2-(2-Piperidyl) Acetamide; 2-Phenyl-2-(2-Piperidyl) Acetic Acid; Series of Benzoic Acid、Benzonitrile; Other pharmaceutical intermediates.

提供盐酸利他林中间体:2-苯基-2-(2-哌啶基)乙酰胺;2-苯基-2-(2-哌啶基)乙酸;苯甲酸、苯甲腈系列及其他医药中间体。

Teflubenzuron was synthesized from 2,4-difluoronitrobenzene and 2,6-dichlobenil as starting reagent through six-step reaction with the yield of 75.3%.3,5-Dichloro-2,4-difluoroaniline was synthesized by chlorination,reduction reaction from 2,4-difluoronitrobenzene,the yield was 84.5%;2,6-difluorobenzamide with the yield of 87.7% was synthesized by fluoridation and hydrolysis from 2,6-dichlobenil.

以2,4-二氟硝基苯和2,6-二氯苯腈为起始原料,经过6步反应合成伏虫隆,总收率为75.3%。以2,4-二氟硝基苯为原料,经过氯化、还原反应合成3,5-二氯-2,4-二氟苯胺,产率为84.5%;以2,6-二氯苯腈为原料,经过氟化和水解,制得2,6-二氟苯甲酰胺,产率为87.7%;将Ⅱ与二碳酸酯酰化,合成2,6-二氟苯甲酰异氰酸酯,产率为91.3%;Ⅲ与Ⅰ加成,得到杀虫剂伏虫隆,产率为95%。

Methods 4-Hydroxybenzonitrile (2) as the starting material was transformed to 4-hydroxy-thiobenzamide (3) via thioformylation. And ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate (4), which was synthesized via cyclization from 3, was treated with hexamethylenetetramine to generate the intermediate ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate (5). The target compound febuxostat (1) was obtained from 5 by etherification, cyanidation, hydrolysis.

以羟基苯腈为原料,经硫代甲酰化得到对羟基硫代苯甲酰胺(3),3经环合得到2-(4-羟基苯基)-4-甲基-噻唑-5-羧酸乙酯(4),4与乌洛托品反应,得到中间体2-(3-甲酰基-4-羟基苯基)-4-甲基-噻唑-5-羧酸乙酯(5),之后再经醚化、氰化、水解得到目标产物(1)。

The results showed that both the break point on the Ia-c curve and the minimum of the derivative variation corresponding to the λa-c curve agreed very well with the critical micelle concentration of the surfactant in aqueous solution as measured by surface tension technique.

以对二甲氨基苯甲腈为探针,测定它在表面活性剂(C12TABr、SDS、C12E23、C12-3-12·2Br)水溶液中的第二重荧光强度和对应的特征波长对表面活性剂浓度曲线,由Ia-c 曲线的转折点或λa-c曲线对应的一阶导数极小点可以获得临界胶团浓度。

Computationalresults indicate that the no-planar trans-benzanilide is the most stable structure. The spectra indicate that the Franck Condon region photodissociation dynamics have multidimensional character withnine activemodes. The intensity of υ24 mode in methanol is much stronger than that in acetonitrile. Compared with fatty amides and benzamide, phenyl substitution for H atom on-NH2 group makes C=O solvent effects disappear.

结果表明,苯甲酰苯胺的非平面反式结构为最稳定结构;在Frank-Condon区域内,苯甲酰苯胺主要由9个活性振动模组成;其中ν24(苯环上C=C不对称伸缩振动和CCH的面内弯曲振动,NH面内弯曲振动)振动模在甲醇溶剂中的强度远远大于其在乙腈的强度;与脂肪酰胺类化合物和苯甲酰胺的研究结果比较发现,苯基取代-NH2上的H原子使得C=O不再具有明显的溶剂效应。

The polymerization of 4,4'-biphenyldicarbonitrilecatalyzed by cuprous chloride was studied.

此外,也研究了以锌和几种不同Lewis酸为催化剂时苯甲腈的聚合反应。

Some useful fluorine-containing intermedi-ates were synthesized by the reaction of activated methylenecompounds or silyl enol ether with 2,2-dihydropolyfluoro-alkanoates or 2-hydropolyfluoroalk-2-enoates in the presenceof different bases.

进一步研究表明,在氢化钠的作用下,苯乙腈,苄基苯基甲酮也可以与2-氢多氟-2-烯酸乙酯发生亲核加成反应,苄基苯基甲酮的加成中间体经多聚磷酸环化,得到了间位氟烷基取代的α-萘酚衍生物。

The latter is chlorinated in the side chains under free-radical conditions to give 2,4-dichloro-5-fluoro-3-dichloromethyl-1-trichloromethylbenzene. The latter is hydrolysed via 2,4-dichloro-5-fluoro-3-dichloromethylbenzoic acid, which can be isolated if necessary, to give 2,4-dichloro-5-fluoro-3-formyl-benzoic acid, the aldehyde group of which is reacted to give 2,4-dichloro-5-fluoro-3-N-hydroxyiminomethyl-benzoic acid, from which, with simultaneous conversion of the carboxyl group into the chlorocarbonyl group, water is eliminated using an acid chloride to give the nitrile 2,4-dichloro-3-cyano-5-fluoro-benzoyl chloride.

随后,在游离基条件下进行侧链的氯化,得到2,4-二氯-5-氟-3-二氯甲基-1-三氯甲基苯、后者被水解,经过2,4-二氯-5-氟-3-二氯甲基苯甲酸(如果需要此化合物可以分离),得到2,4-二氯-5-氟-3-甲酰苯甲酸,将其醛基反应,得到2,4-二氯-5-氟-3-N-羟基亚氨基甲基苯甲酸,用酰氯从其中除去水,同时将羧基转化为碳酰氯,得到一种腈,即2,4-二氯-3-氰基-5-氯-苯甲酰氯。

Methyl phenyl glyoxylate was prepared firstly by reaction of 2-methyl benzoyl chloride with NaCN. The reaction of 2-methyl phenyl glyoxylate with methanol gave the target product methyl 2-methyl phenyl glyoxylate. An improved 3 step synthetic method of methyl 2-methyl phenyl glyoxylate was studied. The optimization conditions were presented.

以2-甲基苯甲酸为原料,酰化后与氰化钠反应生成2-甲基苯甲酰腈,经甲酯化生成2-甲基苯甲酰甲酸甲酯,改进了三步合成2-甲基苯甲酰甲酸甲酯的方法,并对反应时间、反应温度等影响因素进行了优化,确定了合成反应中的最优化条件。

The experiment consist of two parts :the first one research nucleophilic addition of m-dinitrobenzene, nucleophilic reagent is benzyl cyanide; the second one synthesize 2,4-dihydorxybenzophenone from 2,4-dichlorobenzophenone and NaOH.

实验分为两部分:第一部分研究了间二硝基苯的亲核加成反应,亲核试剂为苄基腈;第二部分是用2,4-二氯二苯甲酮与氢氧化钠反应制备2,4-二羟基二苯甲酮。

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