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Ethyloxymethylnaphththyridinecarboxylic acid ; condensation reaction ; cyclization reaction ; ethylation reaction ; hydrolysis reaction ; spectrum characteristic

乙基氧甲基萘啶羧酸;缩合反应;成环反应;乙基化反应;水解反应;光谱特征

The results show that this reaction proceeds in two step: 1 silylene and formaldehyde form an intermediate complex, which is a kind of exothermal reaction with no barrier; 2 the intermediate complex isomerizes to sive the product. The barrier for the second step is 51.4kJ·mol^-^1 at MP2/6-31G^*//6-31G^* level (with zero-point energies correction). In view of dynamics and thermodynamics, it is between 300~400K that the reaction will have not only larger spontaneous tendency and equilibrium constant but also quicker reaction rate.

结果表明,此反应历程由两步组成:1硅烯与甲醛生成一中间配合物,是一无势垒的放热反应,2中间配合物异构化为产物,此步势垒经零点能校正后只有51.4kJ·mol^-^1(MP2/6-31G^*//6-31G^*);从热力学和动力学的综合角度考虑,该反应在300~400K温度下进行为宜,如此,反应既有较大的自发趋势和平衡常数,又具有较快的反应速率。

When The degree of hydrolyzation of oyster protein was 16.39%, and the proportion oyster hydrolysate to the sucrose hydrolysate was 100:3, and the reaction moisture and pH and temperature were 75% and 7.5 and 115℃ respectively, the reaction produced appropriate flavor matters, such as 2-furanmethanol which contributed good flavor to the product, while the reaction time was 0.5h. Maillard reaction was able to conceal fishiness effectively.

结果表明,当牡蛎蛋白质的水解度为16.39%,并按100∶3的比例添加砂糖水解液时,在反应物浓度为25%、pH7.5和115℃条件下反应时间0.5h能生成适量的2-呋喃甲醇等风味物质,产生适度的焦香味,达到比较理想腥味掩盖效果。

The optimum synthetic conditions of hexadecanoic acid diethanolamide used two-step method are as follows:(1)reaction temperature was 140℃, reaction time was 4.5hours and molar ratio of hexadecanoic acid to diethanolamide was 1:1.15.(2)reaction temperature was 80℃, molar ratio of hexadecanoic acid to diethanolamide was 1:1.55 and mass concentration of the catalyst was 0.8%, reaction time was 3 hours.

二步法合成十六酸二乙醇酰胺最佳合成工艺为:(1)反应温度140℃、反应摩尔比n十六酸∶n二乙醇胺=1∶1.15、反应时间4.5h;(2)反应温度80℃、反应总摩尔比n十六酸∶n二乙醇胺=1∶1.55、催化剂用量0.8%、反应时间3h。

The Effect of different reaction conditions (solvent, reaction temperature, molar ratio of iodobenzene and acrylic acid, kind and amount of base, amount of catalyst, reaction time) on the yield was investigated. The suitable condition of the reaction was obtained.

考察了不同反应因素(溶剂、温度、原料比、缚酸剂及其用量、催化剂用量、反应时间)对反应的影响,确定了该催化剂对碘代苯与丙烯酸交叉偶联生成反式-肉桂酸的适宜反应条件。

Synthesis of biodiesel by transesterification of rapeseed oil and methanol catalyzed by KOH/Al2O3 solid base was studied. The catalyst was prepared by isochoric impregnation. Effects of some factors on the transesterification were investigated systematically and reaction conditions were optimized. The optimum reaction conditions on KOH/Al2O3 catalyst were: mass ratio of KOH to Al2O3 20%; calcination temperature 400℃ for 5h; molar ratio of methanol to oil 12:1, the amount of catalyst 5wt%; reaction temperature 60℃ and reaction time 2h.

采用等体积浸渍法制备了KOH/Al2O3负载型固体碱催化剂,并将其用于菜籽油与甲醇酯交换法合成生物柴油的研究;分别考察了催化剂附载量、锻烧温度、醇油摩尔比、反应温度、反应时间等条件对生物柴油产率的影响;结果表明:用等体积浸渍法,在400℃煅烧5h,制得负载量为20%的KOH/Al2O3催化剂。

The method includes steps:(1) dropping triethoxy - 3 - propyl silicane isocyanic acid to ethanol solution of pH sensitive reagent to obtain reaction fluid A;(2) mixing siloxane, acid, and water to obtain reaction fluid B;(3) mixing reaction fluid A, reaction fluid B and solution of calcium chloride according to proportion to obtain solution C;(4) coating solution C on micropore base of micropore plate, using sealing tape to seal micropores, and using needle to perforate each micropore at center, and protecting from light; after placing it a period of time, the method adds distilled water to micropores, keeping the back up.

本发明公开了一种微孔板pH传感器的原位制备方法,其步骤是首先将三乙氧基-3-异氰酸丙基硅烷滴入pH敏感试剂的乙醇溶液中,得反应液A;其次是将硅氧烷、酸和水混合,得反应液B;第三是取反应液A、反应液B及氯化钙溶液,按比例混合,得溶液C;第四是取溶液C涂于微孔板的微孔底部,用密封带将微孔封住,并用针在每个微孔中央刺孔,避光保存。

The dissertation mainly consists of two parts:1. The Reaction Chemistry of Alkynes under Palladium Catalysis Part 1 studies the reaction α,β-unsaturated carbonyl compounds with alkenylpalladium intermediate generated by nucleopalladation, and discovered 1 the Pd-catalyzed tandem addition reaction of halides, alkynes and α,β-unsaturated carbonyls,2 the four-component tandem addition reaction of halides, alkynes and α,β-unsaturated carbonyls, 3 the tandem intramolecular oxypalladation-conjugate additionreaction of alkynoic acids with α,β-enals. These new reactions provide notonly efficient highly stereoselective methods for the synthesis of γ,δ-unsaturated,polyunsaturated carbonyl compounds and γ-lactonic aldehydes, but also thebasic transformations for a number of C-C bond formation reactions which can be usedto design synthesis of many acyclic, cyclic or polycyclic compounds.

本论文的主要工作分为两个部分:一、钯催化下炔烃的反应化学在本小组前人工作的基础上,我们详细研究了炔烃亲核钯化产生的烯基钯中间体与α,β-不饱和羰基化合物的反应,发现两价钯催化下卤离子-炔烃-α,β-不饱和醛酮的串联加成反应、卤离子-炔烃-α,β-不饱和醛酮的西组分串联加成及炔酸分子内氧钯化-串联Michael型加成反应;由此发展了γ,δ-不饱和醛酮、多不饱和羰基化合物和带有醛酮基侧链的γ-丁内酯衍生物的高立体选择性合成方法,这一过量卤离子存在下的烯基钯对α,β-不饱和羰基化合物共轭加成反应的发现,为大量碳-碳键形成反应的实现提供了基础,使我们能够从这一基本反应出发,设计和开发多种分子内、分子间的碳碳成键反应,以好的立体、区域选择性组建开链、环状及多环类型的化合物。

The results show that the optimal parameters of esterification are as follows: 4% of SO42-/ZrO2, molar ratio of methanol to litsea cubeba kernel oil 101, 68 ℃ of reaction temperature and 4 h of reaction time, the acid value decreases to 2.52 mg/g. Compared with the traditional acidic-catalyzed method, this method has the advantages of no acid proof equipment, easy to recycle catalyst and no acidic waste water emission. The optimal parameters of transesterification are as follows: 25 ℃ of reaction temperature, 0.5% of hexadecyl-trimethyl-ammonium bromide, 1% of NaOH, molar ratio of methanol to the oil 61 and 15 min of reaction time. The ester exchanging rate is 97.6%. This method adopts phase transfer catalyst and produces industry prospect, which has many advantages such as energy-saving and time-saving under room temperature.

研究结果表明,固体酸SO42-/ZrO2催化酯化反应的最佳条件为:油重4%的SO42-/ZrO2,醇油摩尔比为101,温度为68 ℃,反应时间为4 h,原油酸值降到2.52 mg/g;该法相对浓硫酸催化酯化法具有不需耐酸设备、催化剂易回收、无废水排放等优点;相转移催化酯交换反应的最佳条件为:温度为 25 ℃,0.5%的十六烷基三甲基溴化铵,油重1%的NaOH,醇油摩尔比为61,反应15 min,原油酯交换率达到97.6%;采用相转移催化技术,反应在常温下进行,大大减少了能耗,缩短了反应时间,具有的产业化前景。

By means of molecular designing, a series of sodium branched-alkyl benzene sulfonates weresynthesized through seven process, involving Frieded-Crafts reaction, Grignard reaction, sulfonationand neutralization. Those isomers have similar structure, carbons of same quantity, but the position ofalkylaryl dissimilarity. Liner fat acid, metaxylene and halogenated hydrocarbon of different carbonnumber were used as the starting materials. Optimum processing condition was confirmed consideringinfluence of a series of reaction factors such as feed proportioning, quantity of catalysts, quantitysolvent, reaction time, temperature and pressure. Eight kinds of isomers of sodium hexadecylxylolsulfonates were finally synthesized, and characterized by FT-IR.

本文通过分子设计,以不同碳数直链脂肪酸、间二甲苯以及不同碳数的卤代烷为原料,经酰基化、格氏反应、加氢还原、磺化及中和等反应,合成了结构相似、烷烃链碳数一定、芳基在烷烃链不同位置的烷基芳基磺酸盐同分异构体;并考察了原料配比、催化剂用量、反应时间、反应温度、溶剂用量、反应压力等一系列因素对各反应的影响,进而确定最佳工艺条件,最终合成出十六烷基二甲苯磺酸钠的八种同分异构体,利用 FT-IR 对产物结构进行了分析。

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