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Synthesis of dimethyl fumarateby esterification of fumaric acid with methanol catalyzed by solid su- peracid SO_4~(2-)/TiO_2was proposed in this paper.

以SO_4~(2-)/TiO_2固体超强酸为催化剂催化富马酸与甲醇合成富马酸二甲酯,探讨了催化剂制备条件、原料配比、反应时间、催化剂用量等因素对富马酸二甲酯收率的影响。

It has offered the information of the boiling points of the chemical compounds, and it is helpful to reutilize them after their separation by rectification. The results showed that the main compounds of the heavy cut of terpineol were longifolene and βcaryophyllene. They are from the raw material, terpinene oil.

松油醇的合成工艺方法主要有两种:一种是一步法,即松节油在酸催化作用下直接进行水合反应生成松油醇;另一种是二步法,即松节油首先在酸催化作用下水合成萜二醇,再经稀酸催化脱水生产松油醇。

To further study the chemical constitutes of lipophilic active parts, we prepared Alc95% and Alc50% according to original literature. 20 compounds were isolated by using macroporous resin, silica gel, polyamide, Sephadex LH-20, Rp-18, preparative TLC and preparative HPLC chromato-graphy. The structures of them were elucidated by means of physical and chemical properties, modern spectroscopic analysis techniques—UV、IR、 EI/MS、ESI/MS、〓H-NMR、〓C-NMR、DEPT、HMQC、HMBC. They are nine anthraquinones: chrysophanol (95-1), physcion (95-2), emodin (95-5), aloemodin (95-7), rhein (50-1), sennoside A or B (50-6),ω-hydroxylemodin (95-10), chrysophanol-8-0-β-D-glucoside (95-12), aloemodin-ω-0-β-D-glucoside (95-13); three phenanthaquinones: tanshinone ⅡA (95-3), cryptotanshinone (95-6), tanshinone Ⅰ(95-4); one isoflavone: 7, 3'-dihydroxyl-5' methoxyisoflavone (95-14) and protocaechuic aldehyde (95-9), protocaechuic acid (95-11), astragaloside Ⅳ(50-4), amygdalin (50-5), 2, 3, 5, 4'-tetrahydroxylstilbene-2-0-β-D-glucoside (50-3),-catechin (50-2), cinnamic acid (95-8). Among them, 3'-dihydroxyl-5' methoxyisoflavone (95-14) is a new compound.

经过溶剂萃取、大孔吸附树脂富集、Sephadex LH-20精制、制备TLC及Semi-pre HPLC等手段从中分离了20个化合物,利用理化性质和波谱技术(UV、IR、EI/MS、ESI/MS、〓H-NMR、〓C-NMR、DEPT、HMQC、HMBC)相结合鉴定了它们的结构,分别为9种蒽醌类化合物:大黄酚,大黄素甲醚,大黄素,芦荟大黄素,大黄酸,番泻苷A或B,ω-羟基大黄素(ω-hydroxylemodin),大黄酚-8-0-β-D-葡萄糖苷(chrysophanol-8-0-β-D-glucoside),芦荟大黄素-ω-0-β-D-葡萄糖苷(aloemodin-ω-0-β-D-glucoside);3种菲醌类化合物:丹参酮ⅡA(tanshinoneⅡA),隐丹参酮,丹参酮Ⅰ(tanshinone Ⅰ);1种异黄酮:7,3'-二羟基-5'-甲氧基异黄酮(7,3'-dihydroxy-5' methoxyisofla-vone)以及原儿茶醛,原儿茶酸,黄芪甲苷(astragaloside Ⅳ),苦杏仁苷,2,3,5,4'-四羟基二苯乙烯-2-0-β-D-葡萄糖苷(2,3,5,4'-tetrahydroxylstilbene-2-O-β-D-g1ucoside),Z—儿茶素,桂皮酸。

In this thesis, investigations focused on heteropoly acids-catalyzed C-C and C-N bond formation reactions and the synthesis of xanthenediones and acridinediones under thermal conditions are described.1.12-Phosphotungstic acid has been used as an efficient,eco-friendly,and air- and moisture-stable catalyst to promote the direct dehydrative substitution of the hydroxy group of benzylic and allylic alcohols with variousβ-dicarbonyl compounds.

本篇论文主要描述了杂多酸催化下的C-C和C-N键的生成,以及无溶剂直接加热下合成十氢氧杂蒽二酮和9-芳基十氢吖啶二酮。主要内容如下:1。在磷钨酸催化下,1,3-二羰基化合物与醇能够顺利偶合,脱除一分子的水,生成烷基化的1,3-二羰基化合物。反应在甲苯中进行时,二芳基甲醇能与各类1,3-二羰基化合物反应,成率很高;但对于1-苯乙醇,只能得到很低的产率。

In this work , 1,8-octodiol, the starting material, reacted with 40% hydrobromic acid to produce 8-bromooctan-1-ol, with the catalytic action of PPTs, its hydroxyl group was protected by 2,3-dihydropyran. Then it coupled with 1-heptaalkyne, by means of P-2 nickel as catalyst, stereoselectivity catalysis hydrogenated, with the catalytic action of acid to take off extremital 2, 3-dihydropyran which protected hydroxy group, then used PCC to oxidize alcohol into corresponding aldehyde.

以1,8-辛二醇为原料,与40%氢溴酸进行单溴代反应,得到8-溴-1-辛醇,在对甲苯磺酸吡啶盐的催化下与2,3-二氢吡喃反应,保护分子中的羟基,再与1-庚炔进行偶联,以P-2镍为催化剂立体选择性催化加氢,酸性条件下脱末端的2,3-二氢吡喃对羟基的保护,使用氯铬酸吡啶盐将醇氧化成醛。

ConclusionThe main components of essential oils are 2,4-bis(1,1-dimethylethyl) phenol (4.4%), tetradecanoic acid (6.96%), n-hexadecanoic acid (7.69%), 9,12-cctadecadienoic acid (6.37%), hexadecanoic acid-2-hydroxy-1- ethyl ester (4.79%) and octadecanoic acid-2-hydroxy-1- ethyl ester (4.77%), respectively.

结论阿给炭挥发油的主要成分为2,4-二树丁基苯酚(4.4%)、十四酸(6.96%)、n-十六酸(7.69%)、-9,12-十八碳二烯酸(6.37%)、软脂酸-2-羟基-1-羟甲基乙酯(4.79%)、硬脂酸-2-羟基-1-羟甲基乙酯(4.77%)。

The obtained CBC was further reacted with stearic acid at 140℃ and hexadecyl alcohol at 180℃ in turn to form citric acid-beta-butylene glycol-citric acidstearic acid-hexadecyl alcohol claw large molecule.

以1,3-丁二醇、柠檬酸为原料,设计、合成了以1,3-丁二醇为核心的柠檬酸-1,3-丁二醇-柠檬酸爪状物小分子;再用酯化反应依次与带有功能化集团的硬酯酸、十六醇接枝合成了多元酯类爪形大分子柠檬酸-1,3-丁二醇-柠檬酸-硬酯酸-十六醇。

Silver nanoparticles with average particle size ranging from 2 to 131nm were manipulatively synthesized starting from silver nitrate using 10 kinds of different functional group-containing organic modifiers, such as polyvinylpyrrolidone, tween-80, sodium dodecyl sulfate, sodium polyacrylate, polyethylene glycol, D-sorbitol, sodium dodecyl sulfonate, sodium dodecylbenzene sulfonate, polyvinyl alcohol, cetyltrimethylammonium bromide, at room temperature.

摘 要:选择10种含有不同官能团的有机物为表面修饰剂,如聚乙烯吡咯烷酮、吐温-80、十二烷基硫酸钠、聚丙烯酸钠、聚乙二醇、山梨醇、十二烷基磺酸钠、聚乙烯醇、十二烷基苯磺酸钠和十六烷基三甲基溴化铵等,在室温下进行了平均粒径在2~131nm范围内纳米银颗粒的控制合成研究。

Monolayer.2. A Novel Sensor Based on Layer-by-Layer Hybridized Phosphomolybdate and Poly on a Cysteamine Modified Gold ElectrodeA novel sensor have been constructed by layer-by-layer hybridizing phosphomolybdate and poly on a cysteamine modified gold electrode.

磷钼杂多酸和聚二茂铁硅烷多层组装膜修饰电极及其电化学行为采用层层组装法在金电极上组装多金属氧酸盐阴离子和聚阳离子聚二茂铁硅烷,交替沉积多层膜,构建了杂多酸-PFS多层膜修饰的金电极。

Study on synthesis of phosphonic acid with thiadiazole and corrosion resistance on copper;2. Synthesis of N,N-dimethyl-1-aminomethane-1,1-di phosphonic acid N-oxide and researches on its corrosion and scale inhibition performances;3. Two phosphonic acid s: dodecylamine-N,N-dimethylene phosphonic acid and dodecyl phosphonic acid,were used to modify zirconia stationary phase in this paper.

通过红外、元素分析对2种不同类型的膦酸化合物改性氧化锆的改性条件和改性机理进行了研究,结果表明:十二烷基膦酸通过Lewis酸碱作用改性,室温浸泡即可达到满意的吸附量;而具有螯合结构的十二胺-N,N-二亚甲基膦酸与氧化锆结合时存在较强的络合作用,最佳改性条件为酸性条件下加热回流。

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