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以p-全氟壬烯氧基苯磺酰氯(Ⅰ)为原料,经酰胺化和季胺化两步反应,制备了N-3-(二甲氨基丙基)对全氟壬烯氧基苯磺酰胺(Ⅱ)和N-[3-(p-全氟壬烯氧基苯磺酰胺基)丙基]-N,N-二甲基乙酸铵(Ⅲ),用FTIR、1HNMR、ESI-MS对II和III的结构进行了表征。中间体N-3-(二甲氨基丙基)对全氟壬烯氧基苯磺酰胺(Ⅱ)的较优合成工艺条件为:溶剂为二氯甲烷,n(Ⅰ):n(N,N-二甲基丙二胺)=1:1.75,20℃反应4 h,Ⅱ的收率可达99.49%。N-[3-(p-全氟壬烯氧基苯磺酰胺基)丙基]-N,N-二甲基乙酸铵(Ⅲ)的较优合成工艺条件为:n(Ⅱ):n(氯乙酸钠)=1:1.1,n(Ⅱ):n(碳酸氢钠)=1:1.5,60℃反应9 h,Ⅲ的收率为93.58%。 相似文献
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以二甲氨基乙醇和丙烯酰氯为原料,制得丙烯酸二甲胺乙酯(DMAEA); DMAEA与1,3-丙磺内酯反应制得甜菜碱型乙烯基两性离子单体--甲基丙烯酰氧乙基二甲基丙磺酸铵(MSBM); MSBM与50%丙烯酰胺水溶液共聚合成了两性聚合物丙烯酰胺/甲基丙烯酰氧乙基二甲基丙磺酸铵(AM/MSBM),其结构经1H NMR和IR确证。研究了矿化度,剪切作用和温度对AM/MSBM粘度的影响。结果表明:AM/MSBM具有反聚电解质溶液行为。在实验条件(盐水矿化度1 075.9 mg·L-1,温度45~75 ℃,剪切速率2 000 rpm)下,AM/MSBM的粘度保持率>90%。模拟驱油实验结果表明,AM/MSBM可提高采收率13.2%。 相似文献
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N-[4-(磺酰胺)苯基]丙烯酰胺(ASPAA)单体可以均聚或与其它单体共聚合成具有药理活性的聚合物,制成水溶性、毒副作用小、具有缓释作用的大分子药物.同时,由于磺酰胺基具有一定的碱溶性,ASPAA与丙烯酸酯类等单体的共聚物可用于制备可碱显影、显影宽容度和耐印力等性能良好的平印、计算机直接制版版材.有关ASPAA与其它单体共聚的竞聚率还鲜见报道.本文在合成ASPAA单体的基础上,对ASPAA/丙烯腈和ASPAA/甲基丙烯酸甲酯共聚的竞聚率进行了研究。 相似文献
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丙烯酰氯的气相色谱分析 总被引:5,自引:0,他引:5
1 引言丙烯酰氯易挥发,暴露于空气与水份作用产生盐酸酸雾,具有强烈的刺激性和腐蚀性.本文用苯胺作衍生反应试剂,使丙烯酰氯与苯胺定量反应生成N-苯基丙烯酰胺,氯化氢与过量苯胺生成氯化苯铵沉淀,从而消除了游离氯化氢对仪器的腐蚀性和给操作带来的不便,再以邻苯二甲酸二异丙酯为内标,经OV-17柱分离,FID检测器测定,实现了丙烯酰氯的无腐蚀简便快速气相色谱分析.2 实验部分2.1 仪器和试剂 GC-9A气相色谱仪(日本岛津公司),FID检测器,CR-3A记录仪.玻璃色谱柱1.1m×3mm,OV-17固定液5%,担体Shimalite W(AW-DMCS)粒径180~154μm.丙烯酰氯对照品98%(贵州省冶金化学研究所).邻苯二甲酸二异丙酯溶液(内标溶液):60g/L苯溶液.苯胺溶液:10%(V/V)的苯溶液.所用溶剂 相似文献
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N-芳基取代的甲基丙烯酰胺(结构式如图1所示)是一类非常有用的共聚单体,它们可以与甲基丙烯酸酯或N-取代马来酰亚胺等单体共聚,使共聚物的一些性能,如耐热性、耐水性、透明度、硬度等都有不同程度的改进[1-4].关于N-芳基取代的甲基丙烯酰胺的制备,文献[5-8]曾有报道,通常采用甲基丙烯酰氯与芳基胺在乙醚、苯等溶剂中反应,并加入适当的缚酸剂来完成.而N-(p-羟基苯基)甲基丙烯酰胺(此处R=OH)是N-芳基取代甲基丙烯酰胺中一种比较特殊的单体,它即含有碳碳双键,又含有酚羟基,属于双官能团物质.关于它的制备及用途,尚未见有文献报道.文献[5]曾报道说,采用对胺基苯酚与甲基丙烯酰氯反应仅能得到甲基丙烯酸(N-(p-甲基丙烯酰胺基)苯酚酯(即酰胺-酯化合物).本文合成出了这种物质,并对其进行了表征和证实;我们推测它与一些单体(如N-取代马来酰亚胺等)的共聚物可以溶于碱性水溶液,并且有好的耐热性,因此在紫外光刻胶中可能有比较大的应用潜力[9-11],有关这方面的内容我们将另文报道. 相似文献
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《合成通讯》2013,43(21):3653-3660
Abstract Silica chloride (SiO2-Cl), as a heterogeneous reagent, has been used for the efficient dehydration of tertiary alcohols under mild reaction conditions. For comparison, we have also used trimethylsilyl chloride (TMSCl) as a homogeneous reagent for this purpose. We have found that silica chloride is a more efficient reagnet than trimethylsilyl chloride for this purpose. Handling of SiO2-Cl is much safer and easier than TMSCl, especially for large-scale operation. The selectivity of the method is also demonstrated by several competitive reactions. Ether formation, rearranged products, and polymerization have not been observed in the reactions. 相似文献
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Chandra S. Sharma Padam N. Nagar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):1793-1798
Dialkyl(aryl) phosphoryl derivatives of alkylene dithiophosphates of general formula (S)SP(O)(OR) 2 : R = Pr i , Ph and G = ═CMe 2 CMe 2 ═, ═CH 2 CH 2 CHMe═, ═CH 2 CH 2 CH 2 CH 2 ═, ═CMe 2 CH 2 CHMe═, and ═CH 2 CMe 2 CH 2 ═; have been synthesized by reacting dialkyl and diaryl phosphoryl chloride with ammonium salts of alkylene dithiophosphates in 1:1 molar ratio in refluxing benzene. The products formed are yellow-colored viscous liquids and white-colored waxy solids; they are soluble in common organic solvents and are nonvolatile, even under reduced pressure. The new compounds have been characterized by elemental analysis, molecular weight measurements and spectroscopic (IR, 1 H NMR, and 31 P NMR)] data. 相似文献
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The sulfenylchlorination of a series of alkenes is investigated by using the combined reagent of dimethyl sulfoxide and oxalyl chloride. The corresponding β-chloro sulfides were obtained in mediate to good yields. Most of the terminal alkenes give the Markovnikov adducts mainly and the sulfenylchlorination of cyclic alkenes is stereospecific to produce the adducts with trans configuration. Methanesulfenyl chloride is supposed to be the real species for sulfenylchlorination. 相似文献
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Cross-coupling reactions of 9-iodo-m-carborane with ferrocenylzinc chloride or cymantrenylzinc chloride catalyzed by (Ph3P)2PdCl2 result in the formation of (m-carbo ran-9-yl)ferrocene and (m-carboran-9-yl)cymantrene, respectively.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 542–543, March, 1998. 相似文献
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IR spectral shifts of carbonyl vibrational absorption for ethyl acetate, which acts analogically as the structural unit of poly(methyl methacrylate), in cyclohexane, chloroform, chlorinated paraffins, poly(vinyl chloride) and chlorinated poly(vinyl chloride) were measured. The results suggest that there are specific interactions between the carbonyl groups and the chlorinated hydrocarbons which could be responsible for the apparent compatibility of poly(vinyl chloride)—poly(methyl methacrylate) and chlorinated poly(vinyl chloride)—poly(methyl methacrylate) blends. Additionally, the effects of the preparation mode of blend films on phase separation and observed compatibility are discussed. 相似文献
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Muhammad Ashfaq 《Journal of organometallic chemistry》2006,691(8):1803-1808
The synthesis of monomer, dimer, tricyclohexyl- and triphenyl-tin(IV) complexes with phthalimido-4-methyl pentanoic acid (PMPA) are described and characterized by FT IR, CHN analyzer, 1H, 13C 119Sn NMR and 119mSn Mössbauer spectroscopic techniques. In vitro ED50, anti-tumor (phytotoxic), anti-yeast, blood pressure and heart rate effect, and bactericidal, fungicidal as well as analgesic bioassays of complexes are also be carried out. The ligand (PMPA) shows excellent analgesic activity while the dimer exhibit strong biocidal and excellent anti-tumor behavior besides of tri-organotin(IV) complexes. 相似文献
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APS引发制备高分子量PDMDAAC 总被引:4,自引:0,他引:4
以已知杂质种类和含量的一步法工业二甲基二烯丙基氯化铵(DMDAAC)单体水溶液为原料,用过硫酸铵(APS)为引发剂,采取低温一次性加入引发剂,分阶段升温方式进行聚合反应,通过合成工艺的优化方法,得到了最高特性黏数值为3.17 dL/g的聚二甲基二烯丙基氯化铵(PDMDAAC),单体转化率为94.8%,采用NMR、IR光谱测试技术对产物进行了结构表征。分别考察了DMDAAC质量分数为57.5%~70.0%、APS与DMDAAC质量比为0.15∶100~0.40∶100、Na4EDTA与DMDAAC质量比为0~0.014 2∶100、聚合反应引发温度T1在40~50℃、聚合反应熟化温度T3在50~90℃范围内的以上5个因素对产物特性黏数和单体转化率的影响规律。结果表明,DMDAAC质量分数为65.0%、APS与DMDAAC质量比为0.35∶100、Na4EDTA与DMDAAC质量比为0.007 1∶100、T1为46℃、T2为50℃,T3为70℃,各反应3 h为最佳工艺条件。 相似文献
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