3,6-位不对称二取代咔唑衍生物的合成研究

以咔唑为主要合成原料,通过N-烷基化、付克酰基化、硝化以及付克烷基化等反应合成了两个结构新颖的3,6-位不对称二取代咔唑衍生物.探讨了原料摩尔比、催化剂用量、反应温度及反应时间等因素对反应的影响,得到最佳反应条件:(1)傅克酰基化反应:n(N-乙基咔唑)∶n(三氯化铝)∶n(乙酰氯)=1∶1.2∶1.5,反应温度室温,反应时间4 h,产品收率82%;(2)硝化反应:n(N-乙基咔唑)∶n(65%硝酸)=1∶1.15,反应温度5~10℃,反应时间2 h,产品收率89%;(3)傅克烷基化反应:n(3-乙酰基-N-乙基咔唑)∶n(氯化锌)∶n(叔丁基氯)=1∶1.5∶1.5,反应温度室温,反应时间12 h,产品收率64%.所得产品结构经FTIR1、H NMR1、3C NMR、及MS表征.     

N-邻苯甲酸基对甲苯磺酰胺的合成

以对甲苯磺酰氯(TSC)和邻氨基苯甲酸(ATRA)为原料,吡啶为溶剂,乙醇钠作催化剂,合成N-邻苯甲酸基对甲苯磺酰胺,采用正交实验设计探讨了投料比、温度、催化剂用量、反应时间对合成反应的影响.最佳的工艺条件是:原料摩尔比n(TSC)∶n(ATRA)=1∶0.6;反应温度35℃;反应时间4 h;催化剂用量为1 g,产品收率大于25%.     

烷基二苯醚双磺酸盐的合成与性能

以α-十二烯、二苯醚及氯磺酸为原料合成十二烷基二苯醚双磺酸盐,对合成过程中的烷基化和磺化反应的工艺条件进行了优化,并用LC/MS进行了表征.单烷基化的较佳反应条件是:反应时间4 h,n(二苯醚)∶n(α-十二烯)=1.0∶1.0,反应温度为70℃,烷基化的产率达88%;磺化的较佳反应条件是:反应时间20 min,n(烷基二苯醚)∶n(氯磺酸)=1∶5,反应温度为10℃,磺酸基的数目为1.86.最后考察了合成样品的表面化学性能及应用性能.     

高收率苄基三乙基氯化铵合成工艺优化

该文研究了以氯苄和三乙胺为原料合成苄基三乙基氯化铵的工艺条件,考察了n(三乙胺)∶n(氯苄)、反应温度和反应时间等因素对反应的影响,通过正交实验优化了合成工艺条件.实验表明:n(三乙胺)∶n(氯苄)为1.0∶1.1,反应温度为84℃,反应时间为2h,苄基三乙基氯化铵收率99％以上.     

一种N,N-二甲基甲酰胺二甲缩醛的温和合成方法

选用新的有机溶剂获得一种N,N-二甲基甲酰胺二甲缩醛(DMFDMA)的温和合成方法,以异构烷烃作为合成DMFDMA的一种新型有机溶剂,考察了反应温度、有机溶剂种类、原料配比、反应时间对产品收率的影响.优化的工艺条件为:第一步反应温度为75℃、异构烷烃作为有机溶剂、n(甲醇钠)∶n(亚胺络合物)=1.2∶1、第二步反应时间是滴加2 h和反应2 h.该条件下,DMFDMA收率达到85.41%,粗产品纯度为97%.采用红外光谱(IR)、核磁分析仪(NMR)、液相色谱-质谱联用仪(LC-MS)对样品进行表征.该合成工艺收率高,操作简单,条件温和,适合工业化生产.     

头孢唑兰活性酯合成工艺改进

在混合溶剂条件下,以亚磷酸三乙酯替代三苯基磷做缩合催化剂,改进头孢唑兰活性酯的合成工艺。经正交实验,考察溶剂、温度和时间等因素对活性酯收率和质量的影响,确定最佳工艺条件为:n(氨噻二唑肟乙酸)∶n(二硫化二苯并噻唑)∶n(亚磷酸三乙酯)=1∶1.1∶1.2,V(二氯甲烷)∶V(乙腈)=1∶1,反应温度为25℃,反应时间4 h。在此条件下,产品收率可达94.8%,HPLC测定纯度为99.2%。     

二苯甲醇的相转移催化合成研究

在相转移催化剂存在下,以二苯甲酮、硼氢化钠为原料合成二苯甲醇,分别研究了反应温度、反应时间、原料配比、催化剂用量等条件对合成反应的影响,确定了最佳工艺条件.该方法合成二苯甲醇的最佳工艺条件是：反应温度25℃,反应时间1 h,n（二苯甲酮）∶n（硼氢化钠）=1∶2.5;相转移催化剂的用量0.6 g、溶剂的用量40 mL（二苯甲酮为0.1 mol的情况下）,二苯甲醇的收率可达到97.56%以上.     

双酚A双(二甲苯基磷酸酯)阻燃剂的合成

利用三氯氧磷、双酚A、苯酚与甲酚反应制得化合物双酚A双(二甲苯基磷酸酯).采用单因素法分别对物料比、反应温度、催化剂进行讨论,确定了适宜的工艺条件:n(三氯氧磷)∶n(双酚A)∶n(苯酚)∶n(甲酚)=3∶1∶2∶4.05;第1步反应温度为50 ℃,反应时间为8 h;第2步反应温度为140 ℃,反应时间为5 h;以AlCl3为催化剂,用量为双酚A总质量的1.5%,产品收率达到87.4%.通过FT-IR对化合物的结构进行了表征,产品质量达到国外同类产品指标;在塑料中添加该化合物,对其阻燃性能进行测试,结果表明这是一种较好的阻燃剂.     

一种糠醛型季铵盐的合成

采用糠醛、正丁胺及卤代烷为原料合成单长链糠醛型季铵盐N-甲基-N-丁基-N-十二烷基-2-呋喃-亚甲基碘化铵,考察了反应时间、物料配比和温度等因素对反应的影响.结果表明N-丁基-2-呋喃-亚胺、N-丁基-N-2-呋喃-亚甲基胺以及N-丁基-N-十二烷基-N-2-呋喃-亚甲基胺的最佳合成条件分别为:反应时间4h,n(糠醛)∶n(正丁胺)=1∶2,反应温度60℃;反应时间4h,n(亚胺)∶n(硼氢化钠)=1∶2.5,温度0～5℃;反应时间16h,n(N-丁基-N-2-呋喃-亚甲基胺)∶n(溴代十二烷)=1∶1.1,反应温度为80 ℃.质谱证实了产品结构,经两相滴定法测得活性物含量为95.1％;产品的cmc为0.000 2moL/L,γcmc为33.93 mN/m,表面活性较好.     

N-月桂酰基乙二胺三乙酸的合成

采用乙二胺和月桂酸为原料,合成N-月桂酰基乙二胺(中间体A),A与一氯乙酸反应得产物N-月桂酰基乙二胺三乙酸(终产物B),通过红外光谱(IR)对合成的中间体N-月桂酰基乙二胺(A)及产物N-月桂酰基乙二胺三乙酸(B)进行结构表征.讨论了反应条件对产率的影响,合成中间体最佳条件为温度110 ℃左右,反应时间约3 h,n乙二胺∶n月桂酸=4∶1.终产物的合成条件为温度80 ℃,反应时间约0.5 h,n氯乙酸∶n中间体=6∶1.     

Markedness and its Interpretation in Language Use

Language markedness is a common phenomenon in languages, and is reflected from hearing, vision and sense, i.e. the variation in the three aspects such as phonology, morphology and semantics. This paper focuses on the interpretation of markedness in language use following the three perspectives, i.e. pragmatic interpretation, psychological interpretation and cognitive interpretation, with an aim to define the function of markedness.     

Features of Women's language

Language is a means of verbal communication. People use language to communicate with each other. In the society, no two speakers are exactly alike in the way of speaking. Some differences are due to age, gender, statue and personality. Above all, gender is one of the obvious reasons. The writer of this paper tries to describe the features of women＇s language from these perspectives： pronunciation, intonation, diction, subjects, grammar and discourse. From the discussion of the features of women＇s language, more attention should be paid to language use in social context. What＇s more, the linguistic phenomena in a speaking community can be understood more thoroughly.     

低渗透非均质砂岩油藏启动压力梯度研究

理论推导与室内实验相结合,建立了低渗透非均质砂岩油藏启动压力梯度确定方法。首先借助油藏流场与电场相似的原理,推导了非均质砂岩油藏启动压力梯度计算公式。其次基于稳定流实验方法,建立了非均质砂岩油藏启动压力梯度测试方法。结果表明:低渗透非均质砂岩油藏的启动压力梯度确定遵循两个等效原则。平面非均质油藏的启动压力梯度等于各级渗透率段的启动压力梯度关于长度的加权平均;纵向非均质油藏的启动压力梯度等于各渗透率层的启动压力梯度关于渗透率与渗流面积乘积的加权平均。研究成果可用于有效指导低渗透非均质砂岩油藏的合理井距确定,促进该类油藏的高效开发。     

On Tragic Consciousness In The Works By Ernest Hemingway

As an American modern novelist who were famous in the literary world, Hemingway was not a person who always followed the trend but a sharp observer. At the same time, he was a tragedy maestro, he paid great attention on existence, fate and end-result. The dramatis personae's tragedy of his works was an extreme limit by all means tragedy on the meaning of fearless challenge that failed. The beauty of tragedy was not produced on the destruction of life, but now this kind of value was in the impact activity. They performed for the reader about the tragedy on challenging for the limit and the death.     

Achieving Unusual States of Matter Under High Pressure

正The periodicity of the elements and the non-reactivity of the inner-shell electrons are two related principles of chemistry,rooted in the atomic shell structure.Within compounds,Group I elements,for example,invariably assume the+1 oxidation state,and their chemical properties differ completely from those of the p-block elements.These general rules govern our understanding of chemical structures and reactions.Using first principles calcula-     

Exchange-Correlation and Electronic Excitation Energies from Pairing Matrix Fluctuations

We have developed an adiabatic connection to formulate the ground-state exchange-correlation energy in terms of pairing matrix linear fluctuations.This formulation of the exchange-correlation energy opens a new channel for density functional approximations based on the many-body perturbation theory.We illustrate the potential of such approaches with an approximation based on the particle-particle Random Phase Approximation(pp-RPA).This re-     

Density Functional Theory for the Response of Periodic Systems to Electric Fields Based on the Vector Potential Approach

正The electronic and nuclear(structural/vibrational)response of 1D-3D nanoscale systems to electric fields gives rise to a host of optical,mechanical,spectral,etc.properties that are of high theoretical and applied interest.Due to the computational difficulty of treating such large systems it is convenient to model them as infinite and periodic(at least,in first approximation).The fundamental theoretical/computational problem in doing so is that     

On the Thermodynamic Limit for Responses to Static Electromagnetic Fields

For molecular systems,the quantum-mechanical treatment of their responses to static electromagnetic fields usually employs a scalar-potential treatment of the electric field and a vector-potential treatment of the magnetic field.Although the potential for each field separately is associated with the choice of an(unphysical)origin,the precise choice of the origin for the electrostatic field has little consequences for the results.This is different for the     

Call for Papers

<正>"The Journal of Shanghai Normal University:Mathematics"is published by Shanghai Normal University as regular issues of The Journal of Shanghai Normal University each year from 2014 in English.The editors-in-chief of the issues are professors Yuhao Cong and Maoan Han.The Journal of Shanghai Normal University was started in 1958 with     

Journal of Donghua University ( English Edition) Contents of Volume 31

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