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We have had the extensive studies on theα-acetyl-α-carbamoyl ketene--acetals and its further applications, for example, their adols condensations with aldehydes giveα-alkenoyl-α-carbamoyl ketene--acetals which can be utilized as the 1,5-bielectronic five-carbon components to react with various binucleophlilic species in a [5+1] annulation.

我们小组在以前的工作中对α-乙酰基-α-胺甲酰基二硫缩烯酮在合成中的应用进行了深入的研究,如与醛缩合生成α-烯酰基-α-胺甲酰基二硫缩烯酮,将其作为1,5-双亲电五碳合成子的[5+1]成环策略等。

The synthesis method comprises the following steps: adding 2-( 5-(dimethylamino methyl- 2- furyl methyl sulpho ethylamine and 1- methylthio- 1- methylamino- 2- nitro ethylene with a molar ratio of 1.04: 1 into water, heating to 48- 52 Deg. C, reacting 4.5 hours with a vacuum degree of 0.02- 0.05 MPa, cooling, adding sodium-hydroxide of concentration of 10% to regulate the PH value to 11.0- 11.4, filtrating and cooling the filtrate to 0- 2 Deg. C, crystallizing for 12 hours, centrifugally filtrating, and rinsing filter cake with purity water to prepare wet ranitidine alkali; dissolving ranitidine alkali in alcohol and reacting with chlorhydric acid to prepare ranitidine hydrochloride.

合成方法包括:将摩尔比为1.04∶1的2-(5-(二甲氨基甲基-2-呋喃基甲基硫代乙胺与1-甲硫基-1-甲胺基-2-硝基乙烯加入水中,升温至48-52℃,于真空度0.02~0.05MPa反应4.5小时,反应完毕降温,用10%氢氧化钠溶液调pH=11.0-11.4,抽滤,滤液降温至0~2℃,结晶12小时,离心甩滤,用纯化水漂洗滤饼,得雷尼替丁碱湿品;将雷尼替丁碱溶于乙醇中与盐酸反应,制备得到盐酸雷尼替丁,产品符合欧洲药典标准。

Chapter two 4-Hydroxybenzoic acid is connected with PEG6000 through defoliant DCC at rooom temperature, then the product is refluxed with chloroacetic acid in acetone to afford PEG-bound phenyloxyacetic acid, which is reacted with thionyl chloride, ammonium thiocyanate and arylamines in turn to give PEG-bound disubstituded thioureas. After the cleavage with sodium methoxide in methanol, the eleven disubstituted thioureas are obtained.

第二章 利用PEG6000作载体,通过脱水剂DCC在室温下将对羟基苯甲酸以酯键连接在PEG6000上,再与氯乙酸在较温和的条件下生成PEG6000支载的芳氧乙酸,然后,依次与亚硫酰氯、硫氰酸铵、芳胺反应,生成PEG6000支载的硫脲,最后用甲醇钠的甲醇溶液切割PEG,得到了十一种1,3-二取代硫脲。

Adenosine was used as the raw material, dissolved in triethyl phosphate and then esterified with thiophosphoryl chloride under 0~5℃ for 8h without water and oxgen, in alkaline condition provided by 2,6-dimethylpyridine, introducing thiophosphoryl ester to adenosine.Then superfluous triethylamine was added and reacted under 5℃ for 1h to synthesize rough 5'-AMPS.The unpurified product was appled to a DEAE Sephadex A-25 column and eluted with triethylammonium bicarbonate.

用腺苷为起始原料,溶解于磷酸三乙脂中后,在无水无氧环境中及2,6-二甲基吡啶提供的碱性条件下与三氯硫磷以0~5℃下发生酯化反应8h,将硫代磷酸酯引入腺苷,然后再与过量三乙胺在5℃下反应1h,合成粗产品,再用碳酸氢三乙胺作洗脱液,过DEAE Sephadex A-25凝胶柱纯化。

By means of covalent coupling with the activation of 1-ethyl-3-(3-dimethyllaminopropyl) carbodiimide hydrochloride and N-hydroxysulfosuccinimide.

利用自组装技术将三巯基丙酸固定在金电极上,以1-乙基-3-(3-二甲氨基)碳二亚胺盐酸盐和N-羟基硫代琥珀亚胺作为活化剂,将甲基对硫磷抗体以共价键形式固定在三巯基丙酸自组装单分子膜修饰的金电极上,制备了一种免疫传感器。

It is characterized in that: 2-( 5-(dimethylamino methyl- 2- furyl methyl sulpho ethylamine reacts with 1- methylthio - 1- methylamino- 2- nitro ethylene directly in water phase, crystallizing and separating out ranitidine alkali.

其特征在于:它是由2-(5-(二甲氨基甲基-2-呋喃基甲基硫代乙胺与1-甲硫基-1-甲胺基-2-硝基乙烯直接在水相中反应并结晶析出雷尼替丁碱。

The results of RT-PCR show that zebrafish treaded TAA 10th day made adipogenetic and lipogenetic up-regulated on the 3th and 5th day, because on TAA treated control Data show that lipogenetic gene would up-regulate at 9th day, so overexpression of PPARγ enhance TAA induced fatty liver.

反转录聚合链反应结果显示转殖PPARγ经TAA处理十天后,在第三有提高的现象,但是从硫乙胺处理控制组的结果显示第9天时,脂肪生成相关基因才会上升,故PPARγ的表现加强了硫乙胺诱导脂肪肝的形成过程。

Two series of polyurethane acrylate grafted acrylic resins (Acr-g-TPU-PETA and Acr-gPPU-PETA) self-emulsifying systems are obtained by grafting -NCO group modified polyurethane acrylates with acrylic copolymer prepared from n-butyl acrylate, styrene,βhydroxyethyl methacrylate and acrylic acid The self-emulsifying systems showed Newtonian fluidity with viscosity closed to that of water, the solid contents were around 30% The T〓 of 15~4℃ for dried film before photocuring favored film formation at room temperature DSC and DMA results showed that PU-PETA is compatible with acrylic resin in the grafted resin The TG and dTG curves for Acr-g-PU-PETA samples were substantially different from the corresponding blends, and the brodened dTG peaks for photocured grafted resin suggest that there might be multiple interactions among chain segments The photocued film of the grafted resins self-emulsifying system exhibited good overall properties with polyurethane acrylate grafts ranging from 30% to 50%, and Acr-g-TPU-PETA series showed better properties than Acr-gPPU-PETA series The adhesion of the photocured film was 1~2 grade, impact strength was 50kg-cm and flexibility was 1mm The Shore hardness and the adhesion of the film decreased markedly if PETA was replaced by HEMA as photoactive group due to the lower C=C double bond content in the grafted resin The polyhydroxy amine-linked thioxanthones photoinitiators can be evenly dispersed in self-emulsifying system without color spot appearing in the dried film The films photocured with IV〓~IV〓 generally exhibited higher Shore hardness, gloss and solventresistance than that cured with Irgacure 2959 and did not induce the rusting of the iron substrate Pigmenting with titanium oxide had no effect on the photocuring The polyhydroxy amine-linked thioxanthone IV〓 and IV〓 can be new candidates for the formulation of titanium oxide pigmented photocurable water-borne coatings for their pale-yellow appearance and slight interference with the color of the coatings WB 4759 with high water-solubility coalesced and separated from the dried resin film, and even induced the rusting of iron substrate.

以丙烯酸丁酯,甲基丙烯酸-β-羟乙酯,丙烯酸及苯乙烯合成厂丙烯酸共聚树脂,并与含-NCO端基的聚氨酯丙烯酸酯接枝反应,经水性化后,得到两个系列(Acr-g-TPU-PETA和Acr-g-PPU-PETA)各5个不同配比的丙烯酸树脂接枝聚氨酯丙烯酸酯自乳化体系,粘度与水相近,为牛顿流体,固含量30%左右。光固化前干燥涂膜的玻璃化转变温度在-15℃~4℃之间,有利于室温下成膜。DSC及DMA谱表明两种树脂基本相容。Acr-g-PU-PETA的热失重行为明显不同于共混材料,接枝样dTG峰明显宽化,表明接枝样中链段之间的相互作刚有多重性,丙烯酸树脂与聚氨酯之间有一定的相容性。接枝树脂自乳化体系光固化涂层的综合性能以聚氨酯丙烯酸酯成分为50%~30%者相对较好,且以Acr-g-TPU-PETA系列更理想。光固化膜的附着力为1~2级,冲击强度为50kg·cm,柔软性多为1mm。以HEMA代替PETA作为接枝树脂的活性基团,碳—碳双键密度太低,光固化膜交联点太少,硬度和附着力均较差。多羟基胺连硫杂蒽酮光引发剂能均匀分散于树脂自乳化体系和接枝树脂干膜中,不出现色斑,光固化膜肖氏硬度一般高于以Irgacure 2959为光引发剂的光固化膜,光泽度及耐丁酮溶剂性能均有所提高,不会诱导铁基生锈,钛白着色对光固化结果几乎没有影响。本论文所合成的多羟基胺连硫杂蒽酮光引发剂IV〓与IV〓为浅黄色,对光固化涂层的颜色干扰较小,为配制钛白着色光固化水性涂料提供了新的光引发剂。水溶性太强的WB 4759在干膜中易聚结析出,且对所附着的铁基有诱导锈蚀作用。

The present invention discloses the structure and application of one new kind of sulphurous heterocyclic naphthyl imides. The said compounds feature that the naphthyl imide has conjugated plane enlarged via the added five- or six-element aromatic heterocycle and introdued sulphurous heterocyclic atom.

本发明公开一类新的含硫杂环并萘酰亚胺化合物的结构及其用途,本发明所说的化合物的特征是萘酰亚胺的共轭平面通过并入的五元芳杂环得以扩大,并引入含硫杂原子。

Tris-(1-aziridinyl)- phosphine oxide and 2-[bis-(2-chloroethyl)-amino]-tetrahydro-1, 3, 2-oxazaphospholidine-2-oxide(Ⅲ, B-518) possess inhibitory action against a variety of animal tumours and have been used clinically. Recently, bis-(1-aziridinyl)-phosphinyl carbamic acid ethyl ester(Ⅱ, AB-100) was found to possess significant activity with low toxicity on experimental animal tumours.

双(2-氯乙基)氨基磷酰二氯与乙烯亚胺在脱水苯或对氧六环中并在三乙胺的存在下进行缩合,生成N,N-双(2-氯乙基)-N′,N-二乙烯基-磷酰胺;与双巯基或双氨基化合物作用,则生成相应的环状磷酰胺、磷酰胺酯以及磷酰胺硫代酯氮芥类化合物。

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