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Orthogonal test was performed to examine the influences of reaction conditions on microwave-assisted synthesis of 2'-oxo-cyclopentanecarboxylic acid ethyl ester from diethyl adipate.

以己二酸二乙酯为原料,在微波辐射下经Dieckmann缩合反应合成2'-羰环戊基甲酸乙酯。

The invention relates to a method for making oligomeric isocyanates by reacting diisocyanates in the presence of a catalyst, wherein the catalyst comprises a saline compound prepared from an anion selected from 1,2,3- or 1,2,4-triazole, a substituted species of 1,2,3- or 1,2,4-triazole and carbocyclically and/or heterocyclically annellated species of 1,2,3- or 1,2,4-triazole and the cation selected from an alkali metal, alkaline-earth metal and/or monovalent ammonium cation and/or phosphonium cation of formula (5), wherein the E, R1, R2, R3, R4 are as defined in the descriotion.

本发明涉及一种制备低聚异氰酸酯的方法,包括二异氰酸酯在催化剂的存在下进行反应,其中所述催化剂由盐化合物组成,该盐化合物由选自1,2,3-或1,2,4-三唑、1,2,3-或1,2,4-三唑的取代系列者、1,2,4-三唑的碳环稠合系列者、1,2,3-或1,2,4-三唑的杂环稠合系列者的化合物及其混合物的阴离子和选自碱金属、碱土金属和/或通式(5)的一价铵阳离子和/或磷友衾胱拥难衾胱又票福其中E、R 1 、R 2 、R 3 和R 4 如说明书中所定义。

Ethyl 4-[(1-hydroxy-1-methyl)ethyl]-2-propyl-1H-imidazole-5-carboxylate,the key intermediate of Olmesartan ,was synthesized from butanoic acid and o-phenylenediamine via condensation under microwave-irradiation,oxidation,esterification and the Gringard reaction.

用正丁酸与邻苯二胺为原料,在微波照射下缩合成2-丙基苯并咪唑,再氧化开环制得2-丙基咪唑二羧酸,再经酯化、Gringard反应制得抗高血压药物奥美沙坦的关键中间体2-丙基-4-[(1-羟基-1-甲基)乙基]-1H-咪唑-5-羧酸乙酯,总收率32.2%。

For developing an immunoassay for multiple residues of pyrethroid pesticides, the hapten N-2- carbanmoyl-(3"-phenoxyphenyl) methyl 3-(2"-Cldoro-3",3",3"-trifluoropropenyl)-2, 2-dimethylcyclopropane- carboxylate was synthesized from cyanohydrin and 3-(2"-Chloro-3",3",3- trifluoropropenyl)-2, 2-dimethylcyclopropanecarboxylic acid via hydrolysis and esterification. The synthesis of the hapten was foundation of preparaing anti- cyhalothrin polyclonal antibodies.

为了制备对单一拟除虫菊酯高特异性的抗体,以菊酸和氰醇为起始原料,通过水解、酯化反应合成了半抗原N-2-氨甲酰-(3-苯氧基苄基)甲基-3-(2-氯-3,3,3-三氟丙烯基)-2,2-二甲基环丙烷羧酸酯,为进一步制备抗三氟氰菊酯的特异性抗体奠定基础。

During the manufacturing of the critical intermediate cephalosporin nucleus --7-amino-3-chloro-cephalosporanic acid diphenylmethyl ester hydrochloride salt, first the feasibility of the one-pot synthetic route of open loop, closed loop and ozonization when chlorine is passed over is qualified by experiments. Then the critical factors that will influence this reaction are studied as follows: the mol ratio of triphenyl phosphite and Diphenylmethyl 3-hydroxy-7-phenylacetaminoceph-3-em-4-carboxylate-l-oxide is four to one; the quantity of the stablizer should be at least more than two to one. The temperature of the system must be 25℃ when chlorine is passed over so that the hydrochloride can be precipitated to obtain cephalosporin nucleus of cefaclor--7-amino-3-chloro-cephalosporanic acid diphenylmethyl ester hydrochloride salt.

在制备关键中间体头孢母核7-氨基-3-氯头孢烷酸二苯甲酯盐酸盐时,先通过实验验证把开环、闭环、臭氧化三步在通入氯气时并为一锅煮的合成路线的可行性之外,又研究了影响该反应的几个重要因素:亚磷酸三苯酯与3-羟基-7-头孢烷-5-亚砜-2-甲酸二苯甲酯的摩尔比为4:1;稳定剂2-甲基-2-丁烯的用量至少大于2:1,通入氯化氢气体时体系温度在25℃时盐酸盐则能够顺利析出,获得头孢克洛的头孢母核—7-氨基-3-氯头孢烷酸二苯甲酯盐酸盐。

Using pentaerythritol as initiator, boron trifluoride diethyl etherate as catalyst.dichloroethane as dispersion agent, the chloride polyether polyol is synthesized based on the mechanism of cationic ring-opening polymerization of epiclilnrohyclrin.The azide polyether polyol is synthesized, in DMF through A and sodium azide, and the non-reported azide energetic curing agent is synthesized through the adduction of B and IIDI.

以季戊四醇为起始剂,三氟化硼乙醚为催化剂,1,2—二氯乙烷为分散剂,环氧氯丙烷经阳离子开环聚合反应制成氯化聚醚多元醇,A在N,N—二甲基甲酰胺中与叠氮化钠反应制得叠氮聚醚多元醇,B与六亚甲基二异氰酸酯加成反应制得未见文献报道的叠氮固化剂。

The main research now is focused on the polymerization of difluoramino substituted oxetane monomers, the preparation of neopentyl difluoramino nitrato plasticizers, and the molecular design and synthesis of cyclic N2 nitramino geminal difluoramino oxidizers.

目前该领域的研究工作主要集中在二氟氨基取代环氧丁烷聚合物合成,新戊基二氟氨基硝酸酯增塑剂制备,以及环N2硝胺基偕二氟氨基氧化剂的分子设计与合成上。

Inside benzene or toluene solvent, in the presence of stannous octoate as catalyst and under the conditions of no water, no oxygen, heating and stirring, MPEG and aliphatic cyclic monomer are ring-opening polymerized to obtain binary block MPEG-aliphatic polyester copolymer.

聚乙二醇单甲醚和脂肪族环酯单体,在苯或甲苯溶剂中,在无水无氧,加热和搅拌的条件下,用辛酸亚锡为催化剂,开环聚合得到聚乙二醇单甲醚-脂肪族聚酯二嵌段共聚物。

A novel method combining a conventional free-radical solution polymerization with a chemical saponification was used to synthesize a, cu-dicarboxyl terminated oligo s with molecular weight below 1500. Here, cn-carboxyl terminated oligo s were firstly synthesized by the free-radical polymerization in THF, where 4,4'-azobis(4-cyanovaleric acid) was used as initiator, thioglycolic acid as chain transfer agent, then CTBMA were transformed into di-CTBMA via saponifying CTBMA in dioxane/H_2O/KOH solution.

利用传统自由基聚合法,在四氢呋喃溶液中自由基引发聚合甲基丙烯酸丁酯单体而得到w-羧基-甲基丙烯酸丁酯低聚物(分子量在1500左右);利用CTBMA 末端酯基的反应特性,在二氧六环/水/KOH混合溶液中皂化CTBMA,使之转化为a ,w-羧基甲基丙烯酸丁酯低聚物;研究了溶剂的类别、反应时间等反应条件对皂化产物结构的影响;利用MALDI-TOF-MS及LSIMS对皂化各阶段产物进行了分析监测。

The optimum conditions for this reaction were confirmed: the mole ratios of the Lewis base and AlCl〓 with the electron-rich aromatic monomer are 1. 2 and 3. 4, respectively; 1, 2-dichloride ethane is the most suitable solvent in this reaction; The solution of the two reactants must be added slowly to a large amount of solvent containing catalyst under pseudo-high dilution conditions; The Lewis base, such as NMP, DMF are applicable in this reaction system.

在此理论的指导下,通过对单体结构的模拟,高选择性地合成了一种新型结构的芳香环状聚硫酯二聚体,对其结构进行了精确的表征,在不同溶剂中得到了该环状二聚体的单晶,单晶X-ray衍射表明该二聚体为环张力极小的大环化合物。

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