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三乙酰胺

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Methods Protein in blood and urine was precipitated directly by acetonitrile with acetanilide was used as the internal standard using Agilent Zorbax SB-Aq column (250 mm×4.6 mm, 5 μm). The mixed solvents of water (triethylamine 0.12%, acetic acid 0.12%) and acetonitrile were used as the mobile phase to separate cephalosporins using gradient elution method at 1 mL/min and 254 nm.

以乙酰苯胺为内标,血液和尿液用乙腈直接沉淀蛋白,采用Agilent Zorbax SB-Aq(250 mm×4.6 mm, 5 μm)色谱柱,流动相选用水(含0.12%三乙胺和0.12%乙酸)和乙腈的混合溶剂梯度洗脱,流速1 mL/min,检测波长254 nm。

By using the a device being similar to water segregator and by controlling the temperature, cyclization of the intermediate product in chloroform reduced carbonization and gave 2-dodecaneanthraquinane in 68.1% yielding.

以十二烷基苯和苯酐为起始原料,经酰基化、关环和磺化三步反应合成了3-十二烷基蒽醌磺酸;并进一步改进和优化了合成工艺条件:即在催化剂三氯化铝过量50%并有三乙胺存在的条件下,中间体2-(4-十二烷基苯甲酰基)苯甲酸收率为72.45%;关环反应采用氯仿作溶剂,利用类似分水器的装置有效控制反应温度以减少碳化,2-十二烷基蒽醌的收率为68.1%。

Acylamino acid-5-fluorouracil were prepared from acylamino acid chlorides and 5- fluorouracil in the presence of 〓.

邻苯二甲酰氨基酸酰-5-氟尿嘧啶则由邻苯二甲酰氨基酸酰氯与5-氟尿嘧啶在三乙胺的存在下制得。

The synthesis of the intermediate amidetriazinone was a crucial step in the synthesis of triazinone. Ethyl acetate was used as the initial material then was carried out for five steps hydrazine hydrate, triphosgene, chloroacetone, hydrazine hydrate respectively with the yield of 59.8%.

三嗪酮类化合物的合成关键是中间体氨基三嗪酮,本文以乙酸乙酯为起始原料,经过酯的肼解、成环反应、胺的烷基化、酮和肼的缩合、酰胺的水解五步反应合成中间体氨基三嗪酮,其收率达59.8%。

Starting with commercial available tosylmethyl isocyanide and but-2-enoic methyl ester, pyrrolo[2,1-f][1,2,4]triazine derivatives was prepared by twelve-steps process in total yiled of 5.0%~8% via pyrrole and pyrrolo [2,1-f] [1,2,4] triazine ring formation, substitution and amination reactions etc.

本文以简单的对甲基苯磺酰甲基乙腈和反-2-丁烯酸为原料,经过形成吡咯,吡咯并[2,1-f][1,2,4] 三嗪环,取代,酰胺化等等12步反应,合成了结构新颖的吡咯并[2,1-f][1,2,4] 三嗪衍生物,总收率达5%~8%。

In the third chapter, the synthesis of5-[(1"S)-1",2"-diacetyl-oxyethyl]-1-phenylpyrazol-3-carboxaldehyde oxime(2) from5-[(1"S)-1",2"-diacetyl-oxyethyl]-1-phenylpyrazol-3-carboxaldehyde(1) and phenyl-hydrazine were introduced firstly. The synthesis of nine dioxapyrrolino[3,4-c]pyrazoles containing chiral pyrazolyl moiety(6a-i) from 2 with N-substituted-phenylmaleimide by nonmetal oxidant IBD-initiated intermolecular 1,3-dipolarcycloaddition was described in detail.

第三章首先以5-[(1′S)-1′,2′-二乙酰氧基乙基]-1-苯基吡唑-3-醛(1)和苯肼为原料,合成了化合物5-(1′S)-1′,2′-二乙酰氧基乙基1-1-苯基吡唑-3-醛-苯腙(2);再用化合物(2)与N-取代苯基马来酰亚胺反应,利用无金属氧化剂—IBD引发1,3-偶极反应,发生分子间的环加成,合成了9种新型手性吡唑连二氧代吡咯啉并

RESULTS: 12 compounds were isolated and identified as aurantiamide acetate (1), aurantiamide benzoate (2), physcion (3), scopoletin (4), vanillin (5), coniferyl aldehyde (6), syringaldehyde (7), syringic acid (8), luteolin (9), apigenin (10), azelaic acid (11), dotriacontanic acid (12), respectively.

结果:从羊耳菊全草的氯仿和乙酸乙酯部分共分离得到12个化合物,分别鉴定为橙黄胡椒酰胺乙酸酯(1),橙黄胡椒酰胺苯甲酸酯(2),大黄素甲醚(3),东莨菪亭(4),香草醛(5),松柏醛(6),丁香醛(7),丁香酸(8),木犀草素(9),芹菜素(10),壬二酸(11),三十二烷酸(12)。

Methods 2-(piperazin-1-yl)-1-(pyrrolidin-1-yl)ethanone (2) was synthesized from pyrrolidine via amidation and substitution, followed by treating with chloroacetyl chloride and triphenylphosphine in a "one pot" manner to give the corresponding phosphonium chloride 3 in a stable and pure form after crystallization from isopropanol.

以四氢吡咯为原料,先与氯乙酰氯成酰胺,再与哌嗪发生取代反应制得中间体[(1-四氢吡咯基)甲基]哌嗪(2);化合物2与氯乙酰氯和三苯基膦反应,经异丙醇重结晶得到稳定的有机鏻盐(3);化合物3与3,4,5-三甲氧基苯甲醛发生Wittig反应,再与马来酸成盐得目标化合物马来酸桂哌齐特(1)。

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。

In this research, liposoluble chlorogenic laurate was synthesized by the acylation with lauroy chloride in the existence of alkali catalyst in non-water phase, and yellowish CGL powders with a yield of 81.24% were obtained under the optimal synthesis conditions determined via single-factor tests and orthogonal experiments, that is, carrying out the acylation at 35℃ for 8h with a n:n: n ratio of 1:1:1.5 and with dimethylformamide as the solvating agent and the thinner.

文中对绿原酸进行了改性,即在碱性催化剂催化的条件下使其与月桂酰氯进行非水相的酯化反应,得到了脂溶性的绿原酸月桂酸酯。经过单因素及正交试验,确定了最佳合成条件为:以N,N-二甲基甲酰胺作为溶解、稀释剂,绿原酸/月桂酰氯/三乙胺的摩尔比为1:1:1.5,温度控制在35℃,反应时间8h。

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