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We investigated constituent of triterpenoid saponins ofAlbizzia, two new compounds together with two known compounds were isolated from Albizzia julibrissin Durazz. by using column chromatography (macroreticular resin, silica gel, Sephadex gel, reverse phase silica gel),preparative HPLC methods et al.On the basis of spectroscopic analysis, including IR,ESI-MS,~1H-NMR,~(13)C-NMR,HMBC,HMQC,~1H-~1HCOSY and chemical methods, the structure of two new compounds were identified as 3 - O -[β-D-xylopyranosyl(1→2)-β-D-fucopyranosyl (1→6)-β- D -2- deoxy - 2 - acetoamidoglucopyranosyl] -21-O-[(6S)-2- trans- 2,6-dimethyl - 6 - O-β- D - quinovopyranosyl -2,7- octadienoyl] - acacic acid- 28 - O-β-D-glucopyranosyl(1→3)[α-L-arabinofuranosyl(1→4)]-α-L-rhamnopyranosyl(1→2)-β-D-glucopyranoside acacic acid 3- O -β- D- glucopyranosy(1→3)-β- D- fucopyranosl(1→6) [β-D- xylopyranosyl (1→2)]-β-D-glucopyranoside ;two known compounds were acacic acid lactone 3- O -β-D- xylopyranosyl-(1→2)-β-D-fucopyranosl (1→6)- 2-deoxy -2 -acetoamido -β-D- glucopyranoside ; acacic acid lactone 3- O-β-D-xylopyranosyl(1→2)-α-L- arabinopyranosl (1→6)- 2- deoxy - 2- acetoamido -β-D-glucopyranoside . The study lays chemical foundation and chemical reference substance for enhancing quality standard of Albizzia julibrissin Durazz.

本研究论文在综述国内外对合欢属Albizzia三萜皂苷化学成分和药理作用研究进展的基础上,利用传统植化分离手段和现代分离技术,包括大孔树脂、硅胶、葡聚糖凝胶、反相硅胶等柱色谱,制备高效液相色谱法等技术从中药合欢皮中分离得到了4个化合物,其中,2个新化合物和2个己知化合物,并进一步通过现代分析技术IR,ESI-MS,~1H-NMR,~(13C-NMR,HMBC,HMQC,~1H-~1HCOSY等和化学方法鉴定了2个新化合物的结构分别是:3-O-[β-D-吡喃木糖基(1→2)-β-D-吡喃夫糖基(1→6)-β-D-2-去氧-2-乙酰氨基吡喃葡萄糖基]-21-O-[(6S)-2-反式-2,6-二甲基-6-O-β-D-吡喃鸡纳糖基-2,7-辛二烯酸基]-金合欢酸-28-O-α-L-呋喃阿拉伯糖基(1→4)[β-D-吡喃葡萄糖基(1→3)]-α-L-吡喃鼠李糖基(1→2)-β-D-吡喃葡萄糖苷,金合欢酸3-O-β-D-吡喃葡萄糖基(1→3)-β-D-吡喃夫糖基(1→6)[β-D-吡喃木糖基(1→2)]-β-D-吡喃葡萄糖苷;2个已知化合物结构分别是:金和欢酸内酯3-O-β-D-吡喃木糖基(1→2)-β-D-吡喃夫糖基(1→6)-β-D-2-去氧-2-乙酰氨基吡喃葡萄糖苷,金和欢酸内酯3-O-β-D-吡喃木糖基(1→2)-α-L-吡喃阿拉伯糖基(1→6)-β-D-2-去氧-2-乙酰氨基吡喃葡萄糖苷。

In this thesis, a convenient and efficient synthesis of highly functionalizeddihydropyrido[2,3-d]pyrimidines via a double [5 + 1] annulation strategy startingfrom easily available α-alkenoyl-α-carbamoyl ketene--acetals 1 and cheapreagents (NH4OAc, DMF, and POCl3) has been developed.

本论文探索了一种简便有效的合成高度官能化的二氢吡啶并[2,3-d]嘧啶的方法,此方法由易得的α-乙酰基-α-氨基乙酰基二硫缩烯酮1和便宜的试剂(醋酸铵,二甲基甲酰胺和三氯氧磷)通过两步[5 + 1]加成而实现。

Results show that, by using thionyl chloride and N,N-dimethyl formamide as chlorinating reagent and dichloromethane as solvent and taking -15℃ as reaction temperature, Z-iomer crystals with pale white color and stable to temperature can be obtained with an overall yield of 70%.

以2-(2-氨基噻唑-4-基)-2-甲氧亚氨基乙酸为原料,经盐酸化、氯代等反应合成了Z-2-(2-氨基噻唑-4-基)-2-甲氧亚氨基乙酰氯盐酸盐;氯代时以用亚硫酰氯和N,N-二甲基甲酰胺的混合物代替五氯化磷作氯化剂,并考察了温度和溶剂对氯代产物中Z-异构体和E-异构体收率的影响。

After the diazotization ,2-aminophenol-4-(2-'carboxy)sulfanil phenylamine was coupled with acetoacetanilide,2-naphthol,1-phenyl-3-methyl-5-pyrazolone,1-naphthol-4-sulfonic acid,separately to get the different diazotized compounds,then complexed with potassium chromium sulfate or cobaltous chloride to obtain the yellow,orange,red,purple,blue and other colour dyestuffs.

2-氨基苯酚-4-(2'-羧基)磺酰苯胺重氮化,分别与乙酰乙酰苯胺、2—萘酚、1-苯基-3-甲基-5-吡唑啉酮、尼文酸、1-乙酰氨基-7-萘酚等偶合,得到不同的偶氮化合物,然后分别与硫酸铬或氯化钴进行络合反应,得到黄、橙、红、紫、蓝多种颜色染料,并进行了毛织品的染色实验。

The synthesis of fructone from ethyl acetoacetate and ethylene glycol using sulfonated activated carbon as solid acid catalyst was investigated.

以活性炭磺化制得新型固体磺酸磺化炭为催化剂,对乙酰乙酸乙酯和乙二醇合成苹果酯的催化工艺进行了系统研究。

The synthesis of l-(4-acetylaminophenyl)-2-bromo-1-propanone was discussed, and the mechanism and possible factors were analyzed. Hence the routine was determined, in which l-(4-acetylaminophenyl)- 1-propanone was reacted with Bromine dissolved in ethanol, so that the a -bromination can be carried on, resulted in the yield of up to 70.4%.

探讨了1-(4-乙酰胺基苯基)-2-溴代-1-丙酮的合成方法,分析了反应机理和影响因素,确定将1-(4-乙酰氨基苯基)-1-丙酮溶解在乙醇中以溴的乙醇溶液进行α-溴化的合成路线,产率可达70.4%。

The α-monobromination of 2-pentone,4-methyl acetophenone,4-methoxyacetophenone,6-methoxy-2-acetylnaphthane,2,2,5,5-tetramethyl-3-hexanone,cyclooctanone,cyclododecanone with respectively,were studied.

研究了离子液体三溴化1-丁基-3-甲基咪唑[Br3]对2-戊酮、4-甲基苯乙酮、4-甲氧基苯乙酮、6-甲氧基-2-乙酰基萘、2,2,5,5-4-甲基-3-己酮、环辛酮、环十二酮、丁醛等羰基化合物的α-溴化反应。

The yield reached 67.0% The medicinal and pesticidal activities of a part of the compounds have been measured .

在进行氨基酰化时,论文克服了该类嘧啶环上4位氨基在常规条件下不与芳香类和带有强吸电子基如三氯乙酰基酰化试剂发生反应的困难,通过采用在强碱性条件下进行酰化,得以成功。

As a key step of the synthesis, the Friedel-crafts acylation was researched. And the optimal operation variables were determined through orthogonal experiment: when 0.lmol acetanilide, 0.26mol aluminum chloride, 0.12mol propionyl chloride and 200ml carbon disulfide are introduced, and the reaction time is 5 hour, the yield can be up to 57.3%. The solid super acid catalyst was preliminary studied. Four solid super acid catalysts were prepared to take the place of aluminum chloride, and it was indicated that AlCl3 acidic resin can better catalyze the Friedel-Crafts reaction of acetanilide.

对合成路线中的Friedel-Crafts酰基化反应进行了研究,运用正交实验设计确定了最佳工艺条件:当乙酰苯胺用量为0.1mol时,AlCl_3用量为0.26mol、丙酰氯用量为0.12mol、溶剂用量为200ml、反应时间为5h,产率可达到57.3%;对于固体超强酸催化剂进行了初步研究,合成了四种催化剂,其中负载AlCl_3强酸性树脂对于乙酰苯胺的Friedel-Crafts酰基化具有一定的催化活性。

acetyl chloride, a novel fluorescence derivatization reagent, has been developed for the determination of sterols and stanol .

采用荧光衍生化试剂2-(9-咔唑)乙酰氯,对天然产物谷甾醇、豆甾醇、菜油甾醇及谷甾烷醇的柱前衍生化条件,包括催化剂的种类、反应温度、衍生化时间等进行了考察,结果表明:催化剂选用三乙胺,反应温度80℃,时间20min,衍生产物具有恒定的最大检测响应值。

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