异丙硫醇的合成研究

研究了以2-溴丙烷和硫脲为原料,在相转移催化剂四丁基溴化铵的作用下,以水作溶剂,制得 S -异丙基异硫脲盐,并在氢氧化钠水溶液中水解,酸化,制得了标题化合物.用气相色谱和红外光谱对其含量和结构进行了分析.     

糠醛异丙硫醇缩醛的合成研究

在１５ｍｍｏｌ对甲苯磺酸催化下,０１ｍｏｌ糠醛和２４ｍｌ异丙硫醇反应得到了糠醛异丙硫醇缩醛,产率７４８％。并通过ＩＲ、１ＨＮＭＲ对产物结构进行了确证。     

异丙硫醇合成反应动力学的研究

研究了硫氢化钠和2-溴丙烷在催化剂作用下合成异丙硫醇的反应动力学,建立了动力学模型.硫氢化钠与2-溴丙烷反应属于一级反应,其化学反应动力学表征方程可表示为:ra=-dca/dt=5.983 34×1012 exp(-11 086/T)ca反应的表观活化能Ea=92.174 kJ·mol-1,并对提出的动力学模型进行了实验验证,两者符合较好.     

苯甲醛异丙硫醇缩醛的合成

苯甲醛和异丙硫醇在对甲苯磺酸催化下发生反应,合成相应的缩硫醛,产率达８４．９％。通过红外光谱、元素分析、核磁共振检测对产物结构进行了确证。     

茴香醛异丙硫醇缩醛的合成研究

茴香醛和惜内硫醇在对甲苯磺酸催化下发生反应,合成阿相应的缩硫醛,产率达８４．９％。通过红外光谱、核磁共振检测,对产物结构进行了确证。     

2—苯基—2—丙硫醇的合成

在催化剂作用下，２－苯基丙烯与硫化氢反应合成了２－苯基－２－丙硫醇，收率８６．６３％，并对反应的影响因素及产物的结构鉴定进行了讨论。     

气相色谱内标定量法分析异丙硫醇含量

以B物质为内标物,利用GC9800TFP型气相色谱仪分析了化学合成的异丙硫醇含量。结果表明：在柱温52℃、汽化室温度150℃、检测器温度200℃、载气流速1mL/min的条件下,色谱分离效果好。相对外标法而言,内标法准确度高,且重复性好。     

气相色谱外标定量法分析异丙硫醇含量

利用GC9800TFP型气相色谱仪分析了化学合成的异丙硫醇含量.结果表明:在柱温50℃、汽化室温度150℃、检测器温度150℃、载气流速1.4 mL/min、分流比50∶1、进样量2 μL的条件下,色谱分离效果好.以峰面积外标法定量,测得精密度实验的标准偏差为7.12×10-4,回收率在98.75%～101.25%之间.外标法不需要校正因子,准确性较高,操作简单,适用于大批量试样的快速分析.     

异丙硫醇产品的红外和核磁共振等的分析

利用元素分析仪、红外光谱仪、核磁共振波谱和气相色谱仪,对以2-溴丙烷和硫脲为原料,通过硫脲法制备的异丙硫醇产品进行了结构表征,结果表明该产品为目的产物,且纯度较高,质量分数可达到99.49％.     

聚硅氧烷丙硫醇铂配合物的合成及应用

合成了一种高分子催化剂聚硅氧烷丙硫醇铂配合物，其用于氢硅化反应时，反应条件温和，反应的总转化率可达65％、90％。该催化剂与同类均相催化剂氯铂酸相比，具有高选择性和稳定性。     

烷基化果胶的合成工艺

为了得到新的结肠靶向给药载体,制备了烷基化甲胶(Alkyl-pectin)。方法:在碱性条件下,以四丁基溴化铵为催化剂,用溴代正辛烷对果胶进行化学改性。结果表明:改性后的果胶是疏水的,并用红外光谱、元素分析、差示扫描量热、核磁共振等方法对产品进行了表征。     

An efficient synthesis of stable sulfur-containing phosphoranes derived from 2-mercapto-1-methylimidazole and 2-thiazoline-2-thiol

Stable crystalline phosphorus ylides were obtained in excellent yields from the 1:1:1 addition reaction between triphenylphosphine and dialkyl acetylenedicarboxylates in the presence of strong SH-acids, such as 2-mercapto-1-methylimidazole and 2-thiazoline-2-thiol. These stable ylides exist in solution as a mixture of two geometrical isomers as a result of restricted rotation around the carbon–carbon partial double bond resulting from conjugation of the ylide moiety with the adjacent carbonyl group.     

2-甲基四氢呋喃-3-硫醇的合成工艺改进

通过优化硼氢化反应条件、2-甲基四氢呋喃-3-硫醇粗品的精馏条件对2-甲基四氢呋喃-3-硫醇的合成工艺进行了改进。改进后的工艺方法简单,所得产品稳定性及收率显著提高,双峰比例一致,可替代进口产品。     

N-烯丙基苯胺的合成研究

以溴丙烯和苯胺为原料合成了N-烯丙基苯胺,通过IR和~1HNMR对化合物的组成和结构进行了表征,探讨了优化反应条件,该路线具有操作简便、反应快、收率高的特点。     

对苯二甲酸二辛酯(DOTP)研制浅析

通过对对苯二甲酸二辛酯(DOTP)两种生产工艺的实验对比、浅析,结和生产实际最后选择采用对苯二甲酸(TPA)法(直接酯化法)生产DOTP。DOTP是聚氯乙烯(PVC)塑料用的一种性能优良的主增塑剂,它与目前常用的邻苯二甲酸二辛酯(DOP)相比,具有耐热、耐寒、难挥发、抗抽出、柔软性和电绝缘性能好等优点。由于(DOTP)不含邻苯二甲酸盐,不在欧盟及其他国家限制使用的16种含邻苯二甲酸增塑剂范围内,是一种优良的环保型增塑剂。     

Catalyst-free sulfa-Michael addition of pyrimidine-2-thiol to nitroolefins

Catalyst-free sulfa-Michael addition of pyrimidine-2-thiol to nitroolefins is described. A series of 2-((2-nitro-1-arylethyl)thio)pyrimidines were efficiently synthesized. The protocol has advantages of wide range of substituents tolerance, no catalyst, additives and bases, mild condition, and high yield. The method can also extend to gram scale.     

Undec-10-ene-1-thiol multifunctional molecular layer as a junction between metallic zinc and polymer coatings on steel

The present work provides the formation of a new duplex system by combination of different layers on steel. Electrodeposition of zinc coating is performed as a first step and serves as a platform for molecular self-assembly and polymer coatings. Undec-10-ene-1-thiol molecule is used as layer junction between zinc surface and the polydimethylsiloxane (PDMS) film. Thiol function interacts by chemisorption with Zn surface while the terminal double bond takes place in the hydrosylilation reaction and thus increases the adhesion of PDMS to the zinc coating. Improvement of corrosion inhibition is evaluated by electrochemical methods at each stage of modification and particularly for the multilayer coating.     

季铵盐在胶束催化肉桂醛水解中的作用

测定了十六烷基三甲基溴化铵(CTAB)胶束体系中不同温度及碱浓度下的肉桂醛水解反应速率,比较了四丁基溴化铵(TBAB)对CTAB、十二烷基硫酸钠(SDS)、聚氧乙烯月桂醚(Brij-35)胶束体系中肉桂醛水解转化率的影响。实验结果表明,当0.003 mol/Lc(CTAB)0.02 mol/L时,肉桂醛水解反应中碱的浓度可从0.1 mol/L下降至0.02 mol/L、反应温度可从318 K下降至298 K,而胶束体系中的反应速率常数基本等于非胶束体系;肉桂醛的转化率(η)依次为η(CTAB+TBAB)η(Brij-35+TBAB)η(CTAB)η(Brij-35)η〔non-(surfactant+TBAB)〕η(SDS+TBAB)η(SDS),且随着TBAB浓度的增加,各胶束体系中肉桂醛的转化率均增大,表明TBAB与胶束催化之间存在着协同作用,它能提高胶束催化的效率。     

Electrochemical study of catechols in the presence of 2-thiazoline-2-thiol: application to electrochemical synthesis of new 4,5-dihydro-1,3-thiazol-2-ylsulfanyl-1,2-benzenediol derivatives

Electrochemical oxidation of catechols (1a–d) has been studied in the presence of 2-thiazoline-2-thiol (3) as a nucleophile in aqueous solution, using cyclic voltammetry and controlled potential coulometry. The results indicate that the quinones derived from catechols (1a–d), participate in Michael addition reactions with 2-thiazoline-2-thiol and via an EC mechanism pathway, convert to the corresponding catechols derivatives (4a–d and 4′d). The electrochemical synthesis of compounds (4a–d and 4′d) has been successfully performed at a carbon rod electrode and in an undivided cell with good yield and high purity. The products have been characterized by IR, ¹H NMR, ¹³C NMR and MS.