N-(2-氯吡啶-3-基)羰基-2''''-取代芳基磺酰胺的合成及除草活性

通过2-氯吡啶-3-甲酸与2-取代芳基磺酰胺的缩合反应合成了6个N-(2-氯吡啶-3-基)羰基-2'-取代芳基磺酰胺化合物,其结构经元素分析、1HNMR、IR确证.初步室内除草活性试验表明,化合物对根、茎的生长均有一定的抑制作用.     

N-（2-氯吡啶-3-基）羰基-2＇-取代芳基磺酰胺的合成及除草活性

通过2-氯吡啶-3-甲酸与2-取代芳基磺酰胺的缩合反应合成了6个N-（2-氯吡啶-3-基）羰基-2＇-取代芳基磺酰胺化合物，其结构经元素分析、^1HNMR、IR确证。初步室内除草活性试验表明，化合物对根、茎的生长均有一定的抑制作用。     

N-(2-氯吡啶-3-基)羰基-2′-取代芳基磺酰胺的合成及除草活性

通过2-氯吡啶-3-甲酸与2-取代芳基磺酰胺的缩合反应合成了6个N-(2-氯吡啶-3-基)羰基-2′-取代芳基磺酰胺化合物,其结构经元素分析1、HNMRI、R确证。初步室内除草活性试验表明,化合物对根、茎的生长均有一定的抑制作用。     

三苯基膦-水体系还原芳基磺酰氯制备芳基硫酚

以甲苯为溶剂,室温条件下,PPh3-H2O体系能够高效并且具有化学选择性地还原各种芳基磺酰氯,生成相应的芳基硫酚。提供了一种反应时间短,以高转化率、高收率制备芳基硫酚的新方法。产物结构经核磁共振光谱、质谱得到了证实。     

1,2-二取代-5-磺酰基咪唑类化合物的制备方法

正本发明属于化合物的合成方法,具体涉及一种1,2-二取代-5-磺酰基咪唑类化合物的制备方法。所述1,2-二取代-5-磺酰基咪唑类化合物的制备方法,是以通式III化合物经5位磺酰化反应获得的通式IV化合物,反应方程式如下:其中R1为烷基或环烷基;R2为烷基或芳基;R3为烷基或芳基。本发明提供的技术方案通过三步反应合成目标产物,总产率超过50%,为前述文献方法     

(E)-β-溴芳基乙烯及芳基乙炔合成方法的改进

(E)-β-溴芳基乙烯和芳基乙炔是重要的有机合成原料及中间体,由于这些原料难以在市场上买到,通常在实验室自己制备。(E)-β-溴芳基乙烯的制备方法主要有：1.由(Z)-β-溴芳基乙烯进行构型转化[1];2.芳基乙烯溴代后,脱去一分子溴化氢,得两种构型的β-溴芳基乙烯[2];3.肉桂酸溴代后,用碳酸氢钠的丙酮溶液脱臭化氢[3]等。芳基乙炔可用芳基溴代乙烯经碱脱去溴化氢而制得[4],也可用芳基乙酮与五氯化磷反应,经脱去氯化氢后制得[5]。我们对上述方法进行了改进,以取代肉桂酸为原料,经纂代,在碳酸钾水溶液中加热脱溴化氢,高产率、高选择性地合成了(E)-β-溴闭幕词基乙烯,后者经三甘醇碱溶液处理,脱去臭化氢,得芳基乙炔。     

手性叔丁基亚磺酰胺的制备方法及其在化学药物合成中的应用价值

本文主要以手性叔丁基亚磺酰胺为研究对象,分析其在合成手性胺类化学药物中的积极作用.本文对手性叔丁基亚磺酰胺的制备方式及其在药物合成的应用状况进行分析讨论,并为该方面相关的药物合成提供了一定的参考价值.     

叔丁基苯氧甲基喹啉酸的一锅法合成及其闭环反应的研究

2-溴甲基-3-喹啉酸乙酯与叔丁基酚发生Williamson反应,反应的中间产物与碱液发牛水解反应,两步一锅法高收率地合成了标题化合物.所得的叔丁基苯氧甲基喹啉酸在Eaton's reagent(P2O5-CH3SO3H)的作用下进行分子内的Friedel-Crafts酰基化反应得到叔丁基取代的苯并杂卓并喹啉酮化合物.化合物叔丁基苯氧甲基喹啉酸、叔丁基取代的苯并杂卓并喹啉酮化合物是未见文献报道的新化合物.它们的结构经红外光谱、核磁共振氢谱和元素分析得以证实.     

吡嘧黄隆及其相关化合物的选择除草活性

磺酰脲类除草剂例如氯黄隆和嘧黄隆为兼具芽前和芽后除草活性的新型化合物(图1),用量极低.笔者对此类化合物的结构及除草活性极感兴趣,正在努力开发兼具高活性和极佳作物安全性的新型化合物.磺酰脲类化合物由三个部分组成:芳基、磺酰脲桥以及杂环(图1).已经了解到芳基能维持除草活性,即使以杂环如噻吩和吡啶替代芳基也是如此.但是,其他部位结构改性一般都降低活性.     

基于芳基肼的苏丹红类染料的合成

旨在开发一种芳基肼与萘酚的偶联反应,实现苏丹红类染料的绿色合成。该反应以对甲苯磺酰氯作为活化试剂,碳酸钾为碱,避免了重氮盐的使用,常温下即可发生,产率较高。反应机理为:磺酰氯与芳基肼反应生成磺酰芳基肼,继而在碱性条件下生成重氮中间体;随后,中间体与萘酚发生偶联反应制得苏丹红类染料分子。创新之处在于,利用磺酰氯活化芳基肼作为重氮源,避免了易暴性重氮盐的使用,使得该方法更加绿色安全。     

肼基甲酸叔丁酯的合成工艺

以氯甲酸苯酯为原料,经过叔丁醇酯化、水合肼肼化得到肼基甲酸叔丁酯,考察了酯化和肼化过程中影响反应的因素。结果表明：酯化反应时间为3 h、反应温度为25～30 ℃条件下,可以得到收率为77%的叔丁基苯基碳酸酯;当水合肼与叔丁基苯基碳酸酯的摩尔比为2∶1,反应温度为100 ℃时,反应产物肼基甲酸叔丁酯的收率可以达到93%,两步总收率为71.7%,其结构经质谱和红外分析确认。     

Epoxidation of chloromethylbutenes by t-butyl hydroperoxide

The epoxidation of chloromethylbutenes by t-butyl hydroperoxide in the presence of Mo(CO)₆ has been investigated. The influence of important parameters on hydroperoxide conversion, selectivity of transformation to epoxy compound in relation to hydroperoxide used, yield in relation to olefin introduced (response function) has been described by regression equations in the form of a second order polynomial. The optimum values of: temperature, olefin to hydroperoxide molar ratio, reaction time, molar ratio of Mo(CO)₆ catalyst to hydroperoxide, ensuring the maximum values of these functions, have been determined. ©1997 SCI     

THE RECOVERY OF METHYL f-BUTYL ETHER FROM CLOSE BOILING IMPURITIES BY EXTRACTIVE DISTILLATION

Methyl t-butyl ether cannot be separated from close boiling compounds by distillation because of the proximity of boiling points. Methyl t-butyl ether can be readily separated from close boiling ethers or hydrocarbons by using extractive distillation in which the extractive agent is dimethylformamide alone or admixed with certain organic compounds.     

Epoxidation of methallyl chloride with t-butyl hydroperoxide

By applying a statistical method of experiment planning the optimum conditions of methallyl chloride epoxidation with t-butyl hydroperoxide have been determined. The influences of the temperature, molar ratio of the methallyl chloride to t-butyl hydroperoxide, catalyst concentration and reaction time on the selectivity of the synthesis of methylglycerol epichlorohydrine in relation to reacted t-butyl hydroperoxide have been examined.     

Parameters of the epoxidation of 1-octene by t-butyl hydroperoxide

The epoxidation of 1-octene with t-butyl hydroperoxide in the presence of Mo(CO)₆ has been studied. The influence of the crucial parameters on the yield of 1,2-epoxyoctane in relation to hydroperoxide, on the hydroperoxide conversion, on the selectivity of the transformation of 1-octene to epoxy compound and on the yield of 1,2-epoxyoctane in relation to 1-octene has been described by the use of regression functions in the form of a second order polynomial. The optimal values of parameters: reaction time, temperature, olefin to hydroperoxide mol ratio, Mo(CO)₆ to hydroperoxide mol ratio, ensuring the maximum values of these functions have been determined.     

连续液相氯化法合成β-氯代特戊酰氯

利用连续液相氯化法对一套间歇氯化法生产β-氯代特戊酰氯的装置进行改造。改造后装置运行情况表明，连续氯化法与间歇氯化法相比，反应时间大大缩短，反应选择性提高，反应收率明显提高。该法可为相同装置或类似的改造提供有益的参考。     

Reactivity of t-butyl chromate resins with substituted α-phenylethanols: A kinetic study

Polystyrene and polyacenaphthylene supports were functionalized to generate a t-butyl chromate function and the resulting polymer-supported reagents were used for the oxidation of alcohols. They were found to oxidize primary and secondary alcohols to the corresponding carbonyl compounds in quantitative yields. Oxidation of differently substituted α-phenylethanols was attempted for this purpose and the kinetics of oxidation reactions was studied. The reaction was found to be first order with respect to the substrate, the reaction being carried out with an excess of the t-butyl chromate reagent. The rate of oxidation was also found to be dependent on the nature of the substrate, concentration of the reagent function, and the nature and concentration of the acid catalyst used. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 67: 799–804, 1998     

Development of a modular microreactor for the partial hydrocarbon oxidation

The industrially important partial oxidation of hydrocarbons is frequently characterized by low conversions and yields, which are mostly related to mass and heat transfer problems. Due to the reaction conditions, such processes include also important safety risks and are still not sufficiently investigated. To study the influence of the process parameters on the product selectivity, a lab facility including a silicon-coated micro reactor of stainless steel has been developed and constructed. Due to its modular construction (e.g., replaceable capillary), it permits for the first time to perform catalyzed and noncatalyzed oxidations of hydrocarbons with oxygen as a two-phase process in a capillary reactor in a wide range of residence times (some minutes to 24?h), temperatures and pressures. Especially wide ranges of reactant ratios and concentrations of inert gas, initiator, and additive are also accessible. The challenges of the reactor construction and their solutions are discussed.     

Gas-phase synthesis of MTBE from methanol and t-butanol over the microporous niobium silicate AM-11

The methyl t-butyl ether (MTBE) synthesis is demonstrated, where MTBE is produced by reacting methanol and t-butanol over the microporous niobium silicate AM-11 (Aveiro Manchester, structure number 11). The effect of the methanol/t-butanol molar ratio, weight hourly space velocity (WHSV) and time on stream (TOS) on this reaction is investigated. These experiments are carried out in the gas phase at temperatures in the range 50–100C and at atmospheric pressure, yielding considerable selectivity for MTBE at low reaction temperatures. The selectivity to MTBE decreases with increasing temperature due to by-products formation. There is no catalyst deactivation during a period of more than 23 h on stream at 70C. Using the catalyst three times has no effect on the catalyst activity and selectivity for MTBE.     

固定化细胞催化合成6-氰基-(3R,5R)-二羟基己酸叔丁酯工艺研究

采用硅藻土作载体,聚乙烯亚胺和戊二醛作交联剂来固定化E.coli BL21(DE3)/pCDFDuet-gdh-cr共表达菌株,以此来催化6-氰基-(5R)-羟基-3-羰基己酸叔丁酯[(5R)-1]合成6-氰基-(3R,5R)-二羟基己酸叔丁酯[(3R,5R)-2],考察了硅藻土-聚乙烯亚胺-戊二醛固定化细胞的催化性能,进一步优化了固定化细胞催化合成(3R,5R)-2工艺。结果表明:在固定化细胞用量100g/L、葡萄糖与底物质量浓度比为1:1、转化温度30℃、pH7.0、流速12mL/min、100 g/L的(5R)-1转化完全的条件下,填充床式反应器可以连续反应五个批次,转化570 g/L的(5R)-1,较搅拌式反应器提高了107.3%,较游离细胞间歇催化操作提高了185%。