苯甲酰胺

Teflubenzuron was synthesized from 2,4-difluoronitrobenzene and 2,6-dichlobenil as starting reagent through six-step reaction with the yield of 75.3%.3,5-Dichloro-2,4-difluoroaniline was synthesized by chlorination,reduction reaction from 2,4-difluoronitrobenzene,the yield was 84.5%;2,6-difluorobenzamide with the yield of 87.7% was synthesized by fluoridation and hydrolysis from 2,6-dichlobenil.

以2，4-二氟硝基苯和2，6-二氯苯腈为起始原料，经过6步反应合成伏虫隆，总收率为75.3%。以2，4-二氟硝基苯为原料，经过氯化、还原反应合成3，5-二氯-2，4-二氟苯胺，产率为84.5%；以2，6-二氯苯腈为原料，经过氟化和水解，制得2，6-二氟苯甲酰胺，产率为87.7%；将Ⅱ与二碳酸酯酰化，合成2，6-二氟苯甲酰异氰酸酯，产率为91.3%；Ⅲ与Ⅰ加成，得到杀虫剂伏虫隆，产率为95%。

Methods 4-Hydroxybenzonitrile (2) as the starting material was transformed to 4-hydroxy-thiobenzamide (3) via thioformylation. And ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate (4), which was synthesized via cyclization from 3, was treated with hexamethylenetetramine to generate the intermediate ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate (5). The target compound febuxostat (1) was obtained from 5 by etherification, cyanidation, hydrolysis.

以羟基苯腈为原料，经硫代甲酰化得到对羟基硫代苯甲酰胺(3)，3经环合得到2-（4-羟基苯基）－4-甲基－噻唑－5-羧酸乙酯(4)，4与乌洛托品反应，得到中间体2-（3-甲酰基－4-羟基苯基）－4-甲基－噻唑－5-羧酸乙酯(5)，之后再经醚化、氰化、水解得到目标产物(1)。

We also found for the first time that the reaction between ketone and alcohol to ketal was catalyzed by benzamide and their derivatives, and the related mechanism is proposed. Furthermore, under the same irradiation condition, the photo-reaction of succimide with alcohol as well as the photolysis of benzene sulfonamide was also found and studied.

并首次发现在紫外光激发下，苯甲酰胺对酮和醇生成缩酮的反应有一定的催化作用，进而对一系列芳酰胺类化合物作了对比实验，发现芳酰胺类化合物均能对缩酮的生成有催化作用，并对芳酰胺的作用机理进行了初步探讨。

They are, 4 21-amidohydrocortisone Ba1～Ba4, 10 21-amidoprednisolone Bb1～Bb10, 4 21-amidomethylprednisolone Bc1～Bc4, 4 21-amidodexamethasone Bd1～Bd4, 1 21-amidobetamethasone Be1, 1 21-amidoRS Bf1, 1 21-amidocortisone Bg1, 1 21-amidoprednisone Bh1. The amido groups were acetamido, nicotinamido, hemesuccinamido, benzoylamido, methanesufonamido, or arylsufonylamido.

包括：4个21-酰胺基氢化可的松（Ba1～Ba4），10个21-酰胺基氢化泼尼松（Bb1～Bb10），4个21-酰胺基甲泼尼龙（Bc1～Bc4），4个21-酰胺基地塞米松（Bd1～Bd4），1个21-酰胺基倍它美松（Be1），1个21-酰胺基RS（Bf1），1个21-酰胺基可的松（Bg1），1个21-酰胺基强的松（Bh1）。21-酰胺基分别为乙酰胺基、烟酰胺基、单琥珀酰胺基、苯甲酰胺基、甲烷磺酰胺基或取代苯磺酰胺基等。

The photocatalytic oxidation performance and kinetics of the simulated organic wastewater in a circulating slurry photocatalytic reactor was investigated.The effects of operation conditions, such as dosage of photocatalyst, illumination time, initial benzamide concentration, pH value, anions and cations in wastewater, on the photocatalytic oxidation performance were discussed.

采用循环式浆态光催化反应器对苯甲酰胺模拟废水光催化氧化特性和动力学进行了研究，系统地考察了操作条件对模拟污染物光催化降解的影响，并与搅拌式和鼓泡床式浆态光催化反应器中苯甲酰胺的降解效果进行对比。

This thesis includes five parts as follows.1. The backgrounds and some relative concepts of this work are briefly introduced. The photochemistry of benzamides and compounds with thiourea functional group is also concisely reviewed.2. Total of fourteen benzamides with different substituted groups have been synthesized and structurally characterized. Better photoreaction time for that kind of compounds at given concentrations is confirmed by tracking its'UV spectrum and GC chromatogram. A representative dibenzophenone photoproduct has been determined by X-ray crystallography. The mechanisms of photoreaction of benzamide have been proposed.3. Total of seven N-chloro(phenylmethylenebenzenamines with different substituted groups and sixty-one thiourea derivatives have been synthesized and structurally characterized.

论文的主要内容如下：1、简要介绍本论文工作的研究背景，并对苯甲酰胺和具有硫脲官能团类化合物的光化学研究进展进行简要的总结。2、合成与表征了14个具有不同取代基的苯甲酰胺类化合物，利用紫外光谱和气相色谱确定了此类化合物较佳光照时间，测定了一个具有代表性光解产物的单晶结构，提出了苯甲酰胺类化合物的光反应机理。3、合成与表征了7个带有不同取代基的氯代苯甲酰亚胺中间体及61个硫脲衍生物，测定了两个具有代表性化合物的单晶结构。

The degradation experiments of benzamide by photocatalysis and electrically assisted photocatalysis demonstrated that the extra electric field had the obvious assistant effect on photocatalysis and the benzamide degradation rate by EAP was much higher than that by photocatalysis. When the electrode potential of photocatalyst was -0.05V/SCE, the removal efficiency of benzamide could be 95% in 120min.

苯甲酰胺降解试验表明，外加电场对光催化氧化技术具有较强的辅助作用，电助光催化氧化技术的处理效率远远高于光催化氧化技术，当施加的电极电位为-0.05V时，苯甲酰胺在120min时的去除率可达95%。

Off-line HPLC coupled with MS gives the result that 4-chlorophenyl urea and 2-chloro-N-(4-chlorophenyl) benzamide are two photoproducts. In comparison with their retention times and UV specta with those of standards, some other photoproducts identified are 2-chloro benzamide, 4-chlorophenyl urea and 4-chloro aniline.

收集光解产物各级分，采用直接进样法在MS上测得其中的二种光解产物为对氯苯基脲和N-邻氯苯甲酰胺：通过与标样在同样HPLC条件下的保留时间和UV吸收光谱相对照，证明产物中存在有邻氯苯甲酰胺、对氯苯基脲和对氯苯胺等。

Computationalresults indicate that the no-planar trans-benzanilide is the most stable structure. The spectra indicate that the Franck Condon region photodissociation dynamics have multidimensional character withnine activemodes. The intensity of υ24 mode in methanol is much stronger than that in acetonitrile. Compared with fatty amides and benzamide, phenyl substitution for H atom on-NH2 group makes C=O solvent effects disappear.

结果表明，苯甲酰苯胺的非平面反式结构为最稳定结构；在Frank-Condon区域内，苯甲酰苯胺主要由9个活性振动模组成；其中ν24（苯环上C＝C不对称伸缩振动和CCH的面内弯曲振动，NH面内弯曲振动）振动模在甲醇溶剂中的强度远远大于其在乙腈的强度；与脂肪酰胺类化合物和苯甲酰胺的研究结果比较发现，苯基取代－NH2上的H原子使得C＝O不再具有明显的溶剂效应。

The photoproducts of CCU in organic solvents have also been identified with HPLC- and GC-MS. The photoproducts identified in methanol are isocyanato bezene, 4-chlorophenyl isocyanate, 2-chloro benzamide, chlorobenzene, 4-chlorophenyl urea, N-phenyl methylcarbamate, N-(4chlorophenyl) methylcarbamate, and 2-chloro-N-(4-chlorophenyl) benzamide.

对灭幼脲在各种有机溶剂中的光解产物作HPLC/UV和GC-MS鉴定，发现其在甲醇中的光解产物含有：异氰酸苯酯、对氯苯基异氰酸酯、邻氯苯甲酰胺、氯苯、对氯苯基脲、N-苯基氨基甲酸甲酯、N-氨基甲酸甲酯、以及N-邻氯苯甲酰胺等。

The reasons of iron ions content overproof in grade Ⅱ desalting water system,such as variation water quality,contamination of regenerant , operation adjustment of pretreatment system and switching operation of bed were discussed.

对二级脱盐水系统中铁离子含量超标的原因，如来水水质发生波动、再生剂受到污染、预处理系统操作调整、床体运行切换等进行了论述。

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