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Whenpyridine was used as reductive decomposing agent, the expecting cholest-4-en-3,6-dione-22-al was obtained. However, when Zn/HOAc was used to decomposethe ozonide, C-4,5 double bond was further reduced to give cholest-3,6-dione-22-al as main product. 2 For the side-chain construction of compound (1), the solid-liquid phase-transfer Wittig reaction was used. When (3-methyl-2-oxobutyl)-triphenylarsonium bromide was used as reagent, the reaction can be carried out inmild reaction condition and the yield is higher than that when phosphorane wasused.

但使用Zn/HOAc作为分解剂时,却得到其氢化产物胆甾-3, 6-二酮-22-醛;2在甾体支链引入过程中,采用固-液相转移Wittig反应的方法,用(3-甲基)-2-氧丁基三苯基溴化胂作为试剂,反应在非常温和的条件下便可完成,而且产率比传统采用膦烷的方法更高;3在对某些甾酮化合物的选择性还原反应研究时,发现在〓还原体系中,当加入某些金属离子后,反应有更好的区域选择性和立体选择性。

While all the phenyl groups in tetraphenylphenyl groups or benzophenanthrene groups are not coplanar. At the same time, by density function theory, the electronic energy gap between HOMO and LUMO frontier molecular orbitals of condensed aromatics are calculated and the Eg of acenaphthenyl groups in C_2 gum is the smallest, which explains the reason why C_2 gum has the best radiation protection effects.

利用甲基三氯硅烷和溴苯的格氏反应合成了甲基苯基二氯硅烷,用核磁分析证实了格氏反应中高沸点副产物为甲基二苯基氯硅烷;通过甲基苯基二氯硅烷和二甲基二氯硅烷的共水解,再裂解而制得含Me_2SiO链节的甲基苯基环硅氧烷混合物,进而利用碱胶开环聚合得到甲基苯基硅橡胶生胶;也可通过甲基苯基二氯硅烷水解所得甲基苯基环硅氧烷D_3~(3Ph、D_4~(4Ph_)与D_4开环聚合制得甲基苯基硅橡胶生胶。

So, by the Diels-Alder reaction of tetraphenylcyclopentadienone, acenaphthenecyclone and benzophenanthrenecyclone with the vinyl groups in C gum, three kinds of polymethylvinylsilicone oil with condensed aromatics are synthesized respectively: polymethylvinylsilicone oil with tetraphenylphenyl groups (called C_1 gum for short), polymethylvinylsilicone oil with acenaphthenyl groups (C_2 gum) and polymethylvinylsilicone oil with benzophenanthrene groups (C3 gum).

根据此原则,利用四苯基环戊二烯酮、苊式环戊二烯酮和菲式环戊二烯酮与C胶上的乙烯基进行Diels—Alder反应,分别合成了三种含稠环基团的乙烯基硅油:四苯基苯基乙烯基硅油(C_1胶),苊式多苯基苯基乙烯基硅油(C_2胶)和菲式多苯基苯基乙烯基硅油(C_3胶),并根据~1HNMR谱图上不同氢原子的积分面积计算了三种胶中稠环基团和乙烯基的含量。

Ten novel derivatives of 1-phenyl-5-[5-(substituted anilinocarbonylmethylthio)-4-phenyl-1,2,4- triazol-3-ylmethylthio]-tetrazole were synthesized rapidly in high yields by the reaction of N--2-chloryacetanilide (3) with 1-phenyl-5-(5-mercapto-4-phenyl-1,2,4-triazol-3-ylmethylthio)-tetrazo- le (2) under microwave irradiation and phase transfer catalysis conditions.

采用微波和相转移催化法通过1-苯基-5-(4-苯基-1,2,4-三唑-5-巯基-3-甲硫基)四唑(2)与2-氯乙酰芳胺(3)反应高效、快速地合成了10种尚未见文献报道的1-苯基-5-[5--4-苯基-1,2,4-三唑-3-甲硫基]四唑。其结构经IR,1HNMR,13CNMR和元素分析表征。生物活性实验结果表明,该类化合物在较低浓度下部分化合物对小麦芽有很好的促进作用

A compound of formula wherein R1 is hydrogen, halo or methoxy; R2 is hydrogen, halo, methyl, ethyl or methoxy; R3 is carboxy, tetrazolyl, or -CONHSO2R where R is methyl, ethyl, phenyl, 2,5-dimethylisoxazolyl or trifluoromethyl; T is -CH2- or -SO2-; and ring A is 3-chlorophenyl, 4-chlorophenyl, 3-trifluoromethylphenyl, 3,4-dichlorophenyl, 3,4-difluorophenyl, 3-fluoro-4-chlorophenyl, 3-chloro-4-fluorophenyl or 2,3-dichloropyrid-5-yl; or a pharmaceutically acceptable salt or prodrug thereof, as well as pharmaceutical compositions containing them are described and claimed.

本发明涉及一种式化合物,其中R 1 是氢原子、卤素或甲氧基;R 2 是氢原子、卤素、甲基、乙基或甲氧基;R 3 是羧基、四唑基或-CONHSO 2 R 4 ,其中R 4 是甲基、乙基、苯基、2,5-二甲基异∴唑基或三氟甲基;T是-CH 2 -或-SO 2 -;环A是3-氯苯基、4-氯苯基、3-三氟甲基苯基、3,4-二氯苯基、3,4-二氟苯基、3-氟-4-氯苯基、3-氯-4-氟苯基或2,3-二氯吡啶-5-基;或其药用允许的盐或前药,还包括所阐述和要求权利的含有它们的药用组合物。

In this article, three novel cyclopalladated ferrocenylimine triphenylphosphine complexes 2-4 were easily synthesized and characterized by elemental analysis, IR, 1H NMR, 31P NMR and X-ray single crystal diffraction.

为筛选高效催化Suzuki反应的催化剂,合成了3种新的环钯化二茂铁亚胺-三苯基膦配合物2~4,经元素分析、红外光谱和核磁共振谱对其结构进行了表征,并通过X射线单晶衍射测定了化合物3的晶体结构。

A synthesis method of 2-(2'-hydroxyl-4'-benzoyloxy-phenyl)-2H-benzotriazole and derivatives thereof is provided, and is characterized in that 2-(2', 4'-dihydroxyphenyl)-5-X-2H-benzotriazole and benzoyl chloride are taken as raw materials for reaction in solvent for 1-8 hours under the temperature of 50-140 DEC C with the mole ratio of 1 to 0.95-1.1, wherein, the amount of the solvent is 2 to 20 times that of the 2-(2', 4'-dihydroxyphenyl)-5-X-2H-benzotriazole and X represents H, F, Cl, Br.

一种2-(2′-羟基-4′-苯甲酸基苯基)-2H-苯并三唑及其衍生物的合成方法,其特征是,以2-(2′,4′-二羟基苯基)-5-X-2H-苯并三唑和苯甲酰氯为原料,在溶剂中进行反应,反应温度50℃~140℃,反应时间1~8小时,反应原料摩尔比2-(2′,4′-二羟基苯基)-5-X-2H-苯并三唑∶苯甲酰氯为1∶0.95~1.1,溶剂用量为2-(2′,4′-二羟基苯基)-5-X-2H-苯并三唑重量的2~20倍,其中X代表H、F、Cl、Br,具有反应条件温和、反应收率高和产物纯度高的特点。

A plausible process of this reaction is as following: Aldehyde was in equilibrium with the enol form, aldehyde reacted with aniline catalyzed by 2,2,2-trichloroacetic acid to afford imine, the generated imine immediately reacted with enol to form intermediate via intramolecular cyclization.

我们发现一分子芳基叠氮和一分子三苯基磷反应生成一分子磷亚胺,后者与由两分子取代的苯氧乙酰氯原位生成的烯酮反应生成4-亚烷基-β-烷基-内酰胺,其串联过程涉及烯酮亚胺的形成及其与烯酮的[2+2]的环加成反应。

A series of sulfonated poly(arylene thioether phosphine oxide)s with various degrees of sulfonation was prepared by polycondensation of 4,4'-thiobisbenzenethiol with the mixture of sBFPPO and BFPPO at different ratios. The effect of IEC on the properties of the products was studied.

以BFPPO、sBFPPO和4,4'-二巯基二苯硫醚为单体,通过改变BFPPO/sBFPPO的配比,合成了一系列不同磺化度的磺化聚芳硫醚三苯基氧膦,考察了IEC对产物性能的影响。

The method comprises: adding 4-(3,4-dichlorophenyl)-1-tetralone and solvent at a ratio of 1:(3-4) into a three-necked flask with a stirrer, heating under stirring until 4-(3,4-dichlorophenyl)-1-tetralone is completely dissolved, heating to 60-100 deg.C, refluxing for 0.5-2 h, cooling the filtrate to -5-10 deg.C, filtering, recrystallizing to obtain refined 4-(3,4-dichlorophenyl)-1-tetralone, and drying at 40-80 deg.C to obtain dry 4-(3,4-dichlorophenyl)-1-tetralone.

该方法的步骤是:在带搅拌的三颈瓶中依次加入4-(3,4-二氯苯基)-1-萘满酮和溶剂,溶剂与4-(3,4-二氯苯基)-1-萘满酮的L∶W为3~4∶1,将上述4-(3,4-二氯苯基)-1-萘满酮及混合精制溶剂搅拌下升温,使4-(3,4-二氯苯基)-1-萘满酮全部溶解,升温至60~100℃,回流0.5-2h;滤液用冰水冷却至-5~10℃,过滤,所得物料再用上述方法进行一次重结晶得到精品4-(3,4-二氯苯基)-1-萘满酮,40~80℃干燥后即得到干品4-(3,4-二氯苯基)-1-萘满酮。

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