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联苯酰

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Starting from 3-benzoyl-5-formyl-indolizine, 3-benzoyl-5-(2'2'-diacetylethenyl)-indolizines and analogs were obtained by the 〓mediated aldol condensation or Wittig reaction. These compounds,promoted by low-valent titanium, gave highly functionlizedcycl[3,2,2]azine derivatives. The coupling reaction proceeded betweenthe carbonyl group and the carbon-carbon double bond, a rare example inMcMurry reaction.

我们以3-苯甲酰基-5-甲酰基中氮茚为原料,通过三碘化钐促进的aldol反应和Wittig反应制备了3-羰基-5-羰基乙烯基中氮茚,随后经低价钛还原偶联,没有生成正常的分子内羰基-羰基偶联产物,而是得到反常的羰基与α,β-不饱羰基的双键偶联产物,较高收率地得到了含多官能团的CycI[3,2,2]azine衍生物。

Three formyl group functional cross-linking polystyrene resins of p -formylphenoxymethyl, p -formyl-2-methoxphenoxymethyl,and p -formyl-3-methoxphenoxymethyl were facilely and rapidly synthesized from Merrifield resin under phase transfer catalytic condition coupling with microwave irradiation in a domestic microwave oven.

以Merrifield树脂为原料,家用微波炉为反应装置,在微波照射的相转移催化条件下,简便快速地合成了3种甲酰基功能化的交联聚苯乙烯树脂——对甲酰基苯氧基甲基树脂、对甲酰基-2-甲氧基苯氧基甲基树脂和对甲酰基-3-甲氧基苯氧基甲基树脂。

Three formyl group functional cross-linking polystyrene resins of methoxphenoxymethyl, and p-formyl-3-methoxphenoxymethyl were facilely and p-formylphenoxymethyl, p-formyl-2-rapidly synthesized from Merrifield resin under phase transfer catalytic condition coupling with microwave irradiation in a domestic microwave oven.

以Merrifield树脂为原料,家用微波炉为反应装置,在微波照射的相转移催化条件下,简便快速地合成了3种甲酰基功能化的交联聚苯乙烯树脂--对甲酰基苯氧基甲基树脂、对甲酰基-2-甲氧基苯氧基甲基树脂和对甲酰基-3-甲氧基苯氧基甲基树脂。

Four non-ionic europium complexes,〓-phen(11),〓·bipy(12),〓·dia(13) and 〓(14)(TTA=2-thenoyltrifluoroacetone, DBM=dibenzoylmethane, phen=phenanthroline, bipy=2,2'-bipyridine, dia=4,5- diazafluoren-9-one, dmbp=4,4'-dimethyl-2,2,-bipyridine), were synthesised and the triboluminescent phenomena of 12, 13 and 14 were firstly observed. Structure determinations of 11,12 and 14 were carried out. The triboluminescence maxima of 12 and 13 are similar to those of their photoluminescence. X-Ray structure analyses show that Eu atoms all exhibit eight-coordinate tetragonal antiprismatic geometries and complexes 11, 12 and 14 are all centrosymmetric.

二、合成了四个非离子型的铕的配合物:〓、〓、和〓(14)[HTTA=2-噻吩三氟甲酰丙酮,DBM=二苯甲酰基甲烷,phen=邻菲罗啉, bipy=2,2'-联吡啶,dia=4,5-二氮杂芴-9-酮,dmbp=4,4'-二甲基-2,2'-联吡啶],首次报道了12、13及14的摩擦发光性质,测定了11、12及14的晶体结构,并系统地讨论了晶体结构和摩擦发光活性之间的关系。12及13的摩擦发光光谱的极大值均类似与其相应的光致发光光谱,表明它们有相同的激发态。

The acetated and hydrogenated urushiol dimer has been separated,and studied by hetero-J resolved 2D-NMR,homo- and heteronuclearchemical shift correlation 2D-NMR and long-range coupled chemicalshift correlation 2D-NMR.The results show that the urushiol dimerare most diphenyl and alkyl phenyl ether structures.Furthermore,IR and MS data also has conformed this structures.

本文将酶催化预聚后的生漆,催化加氢后,乙酰酯化,再进行离心旋转薄层层析,分离得到二聚体主要组分,用异核J分辨谱,同核化学位移相关,异核化学位移相关,远程偶合异核化学位移相关等2D—NMR技术,全面研究了其结构,得到了联苯型和烷基芳醚型聚合结构的结论。

This dissertation is mainly focused on the reactivity of methylenecyclopropanes and comprises six parts. 1 The reactions of methylenecyclopropanes with phenylsulfenyl chloride, phenylselenyl chloride and diphenyl diselenide; 2 The coupling reactions of the ring-opening products derivated from methylenecyclopropanes; 3 The palladium-catalyzed ring-enlargement of mono-aryl group substituted methylenecyclopropanes to cyclobutenes. 4 The gold-catalyzed domino ring-opening and ring-closing hydroamination of methylenecyclopropanes with sulfonamides; 5 The Lewis acid-catalyzed reactions of mono-aryl group substituted methylenecyclopropanes with diethyl ketomalonate in the presence of water; 6 The iodobenzene diacetate mediated novel 1,3-dipolar cycloaddition of methylenecyclopropanes, vinylidenecyclopropanes, and methylenecyclobutane with phthalhydrazine.

本论文主要研究了亚甲基环丙烷类化合物的一些化学反应性能,共由以下六部分组成:1、亚甲基环丙烷类化合物与苯硫氯、苯硒氯及二苯基二硒的反应;2、亚甲基环丙烷类化合物开环产物的偶联反应;3、单芳基取代的亚甲基环丙烷类化合物在钯催化剂作用下的扩环反应;4、金化合物催化磺酰胺对亚甲基环丙烷类化合物的串联开环关环氨氢化反应;5、路易斯酸催化亚甲基环丙烷类化合物与丙酮二羧酸二乙酯在有水存在下的反应;6、醋酸碘苯促进的亚甲基环丙烷类化合物、亚乙烯基环丙烷类化合物及亚甲基环丁烷类化合物与邻苯二甲酰肼的新型1,3-偶极环加成反应。

The structure analysis indicates that the reverse symmetry ligand H4LB molecules are linked into a 2D supermolecular network by two types of hydrogen bonds. One type occurs between the oxalamide oxygen group and the phenol hydroxyl qroup of the nearest molecule with d=2.906(2) and ∠O-H…O=151.8°. The other type is between the oxalamide nitrogen group and the oxalamide oxygen group of anther molecule with d=2.849(2),∠N-H…O=158.7°.

晶体结构研究表明配体H4L为顺式桥联分子,晶体中存在两种氢键,一种是草酰胺基团的O原子与苯环上的酚羟基形成O-H…O氢键[d=2.906(2),∠O-H…O=151.8°];另一种是草酰胺基团的氨基与相邻草酰胺基上的O原子形成N-H…O氢键[d=2.849(2),∠N-H…O=158.7°],通过上述两种氢键将化合物H4LB连接成二维网络结构。

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。

When 3-benzoyl-5-formyl-indolizine or ethyl 5-benzoyl-indolizine-3-carboxylatewere used as substrates, a novel coupling reaction occurred, givinghydroxy-cycl[3,2,2]azines. A mechanism of the reaction was proposed.

其中3-苯甲酰基-5-甲酰基中氮茚和5-苯甲酰基-3-中氮茚甲酸乙酯在低价钛试剂的作用下,发生了新奇的偶联反应,得到了用其它方法难以制备的Hydroxy-cycl[3,2,2]azine,并对此现象作了解释。

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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