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反应制备
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  by reaction
    TiB 2/Al 4.5Cu Composite by Reaction of Mixed Salts in Molten Metal
    盐类反应制备TiB_2/Al-4.5Cu复合材料的研究
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    The Formation of Stable H_4~+ by Reaction
    用离子阱经H_2~++H_2碰撞反应碰撞反应制备H_4~+
短句来源
    Study on the preparation of Fertilizer Containing Nitrogen Sulphur and potassium by Reaction of potassium Chloride and Sulphuric Acid
    氯化钾和硫酸分步反应制备氮钾硫肥的研究
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    Synthesis of Aryl Selenoesters by Reaction of Alkynyl Aryl Selenide and p-Toluenesulfonic Acid
    由芳基炔基硒醚与对甲苯磺酸反应制备芳基硒代羧酸酯
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    The process for the preparation of 2,3-difluoro-5-chloropyridine by reaction of 2,3,5-trichloropyridine with fluoride salts in the presence of phase transfer catalysts is described.
    反应以2,3,5-三氯吡啶为原料,采用KF和CsF的混合物为氟化剂,在一定的条件下反应制备产品2,3-二氟-5-氯吡啶。
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    Si_3N_4 Superfine Powders Prepared by Laser Driven Gas Reaction Method
    用激光驱动气相反应制备Si_3N_4超细粉
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    THE CHARACTERIZATION OF THE CATALYSTS PREPARED VIA A SOLID STATE REACTION FOR PROPANE AROMATIZATION BY USING ESR、IR AND NH_3-TPD
    ESR、IR、NH_3-TPD表征固相反应制备的丙烷芳构化催化剂
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    SYNTHESIS OF NANO-SIZE SIC POWDERS BY LASER DRIVEN GAS PHASE REACTIONS
    激光驱动气相反应制备纳米级SiC超细粉末
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    CHARACTERIZATION BY IR AND AH_3-TPD OF Zn-ZSM-5 CATALYST FOR PROPANE AROMATIZATION PREPARED BY SOLID STATE REACTION
    IR和NH_3-TPD表征固态反应制备的Zn-ZSM-5丙烷芳构化催化剂
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    STUDY ON PREPARATION OF L-PHENYLALANINE BY TRANSAMINASE REACTION
    利用转氨反应制备L-苯丙氨酸
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  by reaction
A series of novel 1,4-bis(p-hydroxyalkoxybenzoate)phenylene were synthesized by reaction of 1,4-bis(p-hydroxybenzoate) phenylene with 3-brompropanol and 4-bromobutanol, respectively.
      
Two novel ferrocenylphenyl-containing amides have been synthesized by reaction of ferrocenylbencarboxylchloride and 1, 2-di-(o_aminophenoxy)ethane.
      
On the Involvement of the Water-Polaron Mechanism in Energy Trapping by Reaction Centers of Purple Bacteria
      
Tagging of η mesons is performed by detecting 3He ions produced by reaction pd → 3Heη close to the production threshold.
      
Determination of Chloroacetic Acids in Drinking Water by Reaction Gas Chromatography
      
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(1) Amidophosphorates (II) could be obtained directly from the reaction of a secondary phosphite (I) with amines in the presence of carbon tetrachloride. This method could be slightly modified as follows:(a) The process was carried out without isolating the intermediate (I) by adding phosphorus trichloride to a mixture of alcohol and carbon tetrachloride and treating the crude product directly with amine.(b) Compounds (II) could be prepared by adding concentrated potassium hydroxide solution to a mixture of...

(1) Amidophosphorates (II) could be obtained directly from the reaction of a secondary phosphite (I) with amines in the presence of carbon tetrachloride. This method could be slightly modified as follows:(a) The process was carried out without isolating the intermediate (I) by adding phosphorus trichloride to a mixture of alcohol and carbon tetrachloride and treating the crude product directly with amine.(b) Compounds (II) could be prepared by adding concentrated potassium hydroxide solution to a mixture of (I), amine salt and carbon tetrachloride, instead of using free amine directly.(2) In the preparation of amidophosphorates (III) granulated sodium or potassium hydroxide, instead of dimethyl cyclohexyl amine, could be used as auxiliary base.(3) In an attempt to prepare the alkyl ester of dialkyl amidochlorophosphoric acid by heating alkyl dichlorophosphate with dried dialkylamine hydrochloride, instead of the desired product (VII), a resinous substance was obtained. It has been assumed that the first produced compound (VII) was polymerized by heating.

(一)利用二代亚磷酸酯(Ⅰ)与四氯化碳及强硷性胺的反应制备化合物Ⅱ,并简化制备过程。 (二)用价廉易得的氢氧化钠(或钾)的颗粒替代辅助剂二甲基环六烷胺,使弱硷性胺如苯胺亦能与Ⅰ和四氯化碳反应。 (三)拟用盐酸二甲基胺盐和Ⅳ共热制备Ⅶ;但仅得一胶状物。此物用五氯化磷处理得Ⅴ。

Seventeen new substituted 3-dialkylaminomethyl-thiochroman have beenprepared by means of the Mannich reaction. The majority of those compoundswere used for the purpose of the testing chemotherapeutic activity towardSehistosomiasis Japonica in experimantally infected animals.Under the same conditions (reacting temperature and duration of reaction),the four substituted (6-Nitro-; 6-Acetamino-; 6-MethoXy- and 7-Acetamino-)thiochromanones were reacted with five Mannich reagents respectively. Thefive Mannich reagents...

Seventeen new substituted 3-dialkylaminomethyl-thiochroman have beenprepared by means of the Mannich reaction. The majority of those compoundswere used for the purpose of the testing chemotherapeutic activity towardSehistosomiasis Japonica in experimantally infected animals.Under the same conditions (reacting temperature and duration of reaction),the four substituted (6-Nitro-; 6-Acetamino-; 6-MethoXy- and 7-Acetamino-)thiochromanones were reacted with five Mannich reagents respectively. Thefive Mannich reagents were bis-(dialkylamino-) methane with small quantity ofthe corresponding amine hydrochloride (method A); bis-(dialkylamino-) methaneonly (Method B); amine hydrochloride with paraformaldehyde in acid medium(pH 3--4) (method C); piperidine with paraformaldehyde (method D), andpiperidine, paraformaldehyde with small quantity piperidine hydrochloride(method E). It was found that rnethod A gave much better results than allthe others, and better results were obtained by using of the method B thanC, D and E in differant degree. More dimers, which were polymerized fromthe decomposed products of Mannich bases during the reaction, were obtainedby means of the method E than the others (see table 1 and 2 in Chinese text).The favorable condition for method A was also discussed.

本文应用 Mannich反应制备十七种3-二烃氨基甲基-苯并硫六圜-4-酮衍生物。首先选择四种苯并硫六圜-4-酮衍生物(Ⅳ,6-NO_2~-,6-CH_3CONH-,7CH_3CONH-6-CH~3O-)在同一条件下(反应温度和时间),用五种不同方法进行反应,即双-(二烃氨基)-甲烷和少量相当胺的盐酸盐(甲法);只用双-(二烃氨基)-甲烷(乙法);胺的盐酸盐和聚甲醛在酸性溶液中(pH=3—4)反应(丙法);六氢吡啶和聚甲醛(丁法)以及六氢吡啶,聚甲醛与少量六氢吡啶盐酸盐(戊法)。亦用甲,乙、丙三法对其他的苯并硫六圜-4-酮衍生物进行反应。比较结果,以甲法所得 Mannich 碱盐酸盐的产量最高,乙法亦比丙、丁、戊三法所得产量高。如以在反应中 Mannich 碱分解后而形成的二聚物得量计,则以戊法为最显著,丁法次之。应用甲法进行 Mannich 反应的优点亦有讨论。

1. In the well-known Stephen method of preparing aldehydes from cor-responding nitriles by reducing the latter with anhydrous stannous chloride inthe presence of hydrogen chloride in anhydrous ether, two typical nitriles,namely, toluonitrile and a-naphthonitrile, could not be reduced smoothly andgave negligible yields. This was ascribed by previous authors to the sterichindrance in the classical sense of the words. We have now carried out moreextensive research, subjeeting variously ortho-, meta-, and para-substitutedhalo-,...

1. In the well-known Stephen method of preparing aldehydes from cor-responding nitriles by reducing the latter with anhydrous stannous chloride inthe presence of hydrogen chloride in anhydrous ether, two typical nitriles,namely, toluonitrile and a-naphthonitrile, could not be reduced smoothly andgave negligible yields. This was ascribed by previous authors to the sterichindrance in the classical sense of the words. We have now carried out moreextensive research, subjeeting variously ortho-, meta-, and para-substitutedhalo-, methoxy-, and carboethoxybenzonitriles to the reduction process underidentical conditions and by comparing the yields obtained with various resultingsubstituted benzaldehydes (see Table I), and found that steric hindrance cannot be regarded as the sole cause which prevents Stephen reaction to proceedsmoothly. In view of the fact that 2, 6-dichlorobenzonitrile and 2, 6-dimethoxy-benzonitrile failed to be reduced completely, steric hindrance must play animportance part in the process. There must be other factors which share withthe steric hindrance in the reaction but their characters are not yet ascertained. 2. Most of the substituted benzonitriles used were known and preparedpreviously by dehydration of the corresponding benzamides or by halogenationof benzonitriles. In both of the processes, the yields were not satisfactoryand the products were not always pure enough. We prepared the necessarysubstituted benzonitriles by Sandmeyer reaction from the corresponding aminesand found that this route gave satisfactory yields and purer products. 3. Though the substituted benzaldehydes prepared in the present workare all known compounds, but only a few of these were previously prepared bythe Stephen method. 4. The attempted reduction of pentaacetyl-D-glucononitrile to pentaacetyl-D-aldehydo-glucose failed; the product was pentaacetyl-D-gluconamide.

1.将各种邻、间、对位由卤素、甲氧基、酯基取代的苯甲腈,用Stephen反应还原,在相同的试验条件下,析离还原后水解得到的醛,比较产率。空间阻碍并不是限制Stephen反应顺利发生的唯—原因,但2,6-二氯苯甲腈和2,6-二甲氧基苯甲腈不能还原的事实说明空间阻碍确有一定作用。 2.本研究所用的芳基甲腈由相应的芳胺,经Sandmeyer反应制备,产率颇好,产品亦纯。许多由芳基甲腈还原生成的芳醛也都是已知的化合物,但有些过去未曾用Stephen反应制备过。 3.用Stephen法还原五乙酰葡萄糖腈,得到的是五乙酰葡萄糖酰胺。

 
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