氯乙酸

Methods 4-Hydroxy- benzonitrile was treated with sodium hydrogen sulfide and anhydrous magnesium chloride in dimethyl formamide to give thioamide, which was then directly cyclized with ethyl 2-chloroacetoacetate without separation to give ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(2) in one-pot; then 2 was formylated with Duff reaction adopting hexamethylenetetramine in trifluoroacetic acid to give ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(3); finally, the target compound was obtained by the treatment of 3 with hydroxylamine hydrochloride and sodium formate in formic acid.

采用"一勺烩"方法，以4-羟基苯甲腈为起始原料，首先与硫氢化钠和无水氯化镁在N，N-二甲基甲酰胺中反应，所得中间体不经分离，直接加入2-氯乙酰乙酸乙酯进行环合反应，得到2-(4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯（2）；然后通过六亚甲基四胺/三氟乙酸进行Duff反应，得到2-(3-甲酰基-4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯（3）；再经盐酸羟胺/甲酸/甲酸钠体系脱水得到目标化合物。

And the optimum pH was 4-6 for the dechlorination reaction of 2,4-D, and pH between 2 and 8 were all suited for the reaction in Pd/Fe systems. Intermediate and final products of 2,4-D, HCH and chlordane with Pd/Fe were determined by GC/MS, and the possible dechlorination pathways were concluded: 2,4-D can be converted to phenoxyacetic acid through gradual hydrogenolysis, and HCH can be transformed to cyclohexatriene through dichloroelimination or dehydrochlorination.

通过GC/MS定性定量分析了三种目标污染物在Pd/Fe体系中发生还原脱氯反应过程中的反应物及最终产物，并根据反应产物推测分析了这三种有机污染物在催化还原反应体系中可能的反应途径：2，4-D主要通过逐级氢解最终生成彻底脱氯产物苯氧乙酸；而六六六则可能通过逐步双氯消除反应或脱氯化氢反应，最后生成环己三烯。

The results showed as follows: 1 Extraction of gelsemium total alkaloids. Total alkaloids were extracted with 95 per cent ethanol. The extract rate was 0.519 per cent and the extract purity were 88.02 per cent and 87.38 per cent; Total alkaloids were extracted with chloroform .The extract rate was 0.416 per cent and the extract purity were 89.02 per cent and 94.52 per cent. 2 Isolation of gelsemium total alkaloids with TLC. Total alkaloids contained five or more alkaloids. The optimal developing agent was chloroform :methanol :ethyl acetate(9:l:0.3),the optimal eluent was methylene chloride:methanol(92:8). 3 Isolation of total alkaloids with column chromatography. Alkaloid A and alkaloid B were obtained, alkaloid B was identified as koumine.

研究结果如下：1、钩吻总碱的提取：用95％的乙醇提取钩吻生物碱提取率为0.519％，其提取物纯度为88.02％、87.35％；用氯仿提取钩吻生物碱提取率为0.416％，其提取物纯度为89.02％、94.52％。2、钩吻总碱的薄层层析分离：总碱中含有5种或5种已上的生物碱；氯仿：甲醇：乙酸乙酯(9：1：0.3)是最佳薄层层析的展开剂；二氯甲烷：甲醇(92：8)是柱层析的最佳洗脱剂。3、钩吻总碱的柱层析分离：共得到两种钩吻生物碱单体成分碱A和碱B，碱B为钩吻素子，碱A可能是钩吻素甲。4、钩吻总碱的急性毒性试验：钩吻总碱小鼠腹腔注射的半数致死量LD_(50是：7.38mg／kg，95％的可信限范围为：6.67mg／kg～7.94mg／kg。

Dichlorophenoxyacetic acid (2,4-D), a widely used herbicide, was treated by the ozonization technology in the laboratory.During the 2,4-D ozonization, the main categories of intermediates included chloric aromatics, dechlorinated aromatics and organic acids.Some of these intermediates have relatively high toxicity.Therefore, it is crucial to study the kinetics trend of intermediates diversion.

采用臭氧化高级氧化技术对2，4-D（2，4-二氯苯氧乙酸）污染物进行降解，2，4-D降解过程中会产生含氯芳香中间产物、无氯芳香中间产物和有机酸类中间产物，其中部分中间产物具有较高毒性，因此研究2，4-D臭氧化过程中间产物的动力学变化趋势是非常重要的。

A novel compound——N-naphthalene acylN′-substituted p-chlorobenzamido thiocarbamide was synthesized by reaction of p-chlorobenzamido hydrazine and α-naphthalene acyl mustard oil,which was obtained by potassium thiocyanate combined with α-naphthalene acyl chloride formed from α-naphthylacetic acid and SOCl2 in anhydrous benzene.

通过α-萘乙酸和SOCl2在无水苯中反应制得α-萘乙酰氯，然后与硫氰酸钾反应生成α-萘乙酰基异硫氰酸酯，再与对氯苯甲酰肼进行加成反应，合成了新型化合物N-萘乙酰基-N′-对氯苯甲酰氨基硫脲，用薄层色谱法跟踪最后一步反应，确定了反应时间。

Naphthalene acetyl chloride was prepared firstly by the reaction between α-naphthylacetic acid and SOCl2 in anhydrous benzene,then reacted with potassium thiocyanate to obtain α-naphthalene acetyl isosulfocyanate,as taking an addition reaction with p-chloro benzoyl hydrazine the novel compound N-naphthalene acetyl-N'-p-chloro benzoylamino thiocarbamide was finally synthesized.

通过α-萘乙酸和SOC l2在无水苯中反应制得α-萘乙酰氯，然后与硫氰酸钾反应生成α-萘乙酰基异硫氰酸酯，再与对氯苯甲酰肼进行加成反应，生成新型化合物N-萘乙酰基-N'-对氯苯甲酰氨基硫脲。

New ruthenium benzylidene complexes benzylidene[1,3-bis(2,6-dimethylphenyl)-4,5-dihydroimidazol-2-ylidene] [k~2-diphenylphosphinoacetato] monochlororuthenium (46), benzylidene[1,3-bis(2,6-dimethylphenyl)-4,5-dihydroimidazol-2-ylidene][k~2-3-propionato]monochlororuthenium (47), benzylidene[1,3-bis(2,6-dimethylphenyl)-4,5-dihydroimidazol-2-ylidene] [k~2-2-benzonato]monochlororuthenium (48) featured five-membered, flexible six-membered and rigidsix-membered chelating rings respectively are prepared by reactions of complex 41 withcorresponding sodium phosphino-carboxylates. It is confirmed by X-ray crystallographicanalysis that the coordination geometries of complexes 46 and 47 are distorted squarepyramids with phosphino-carboxylate ligands chelating to ruthenium, and the coordinationbetween ruthenium and benzylidene ligands are strengthened.

用二苯基瞵乙酸盐、二苯基膦丙酸盐、二苯基膦苯甲酸盐与钌卡宾配合物41反应合成了三个新的钌卡宾配合物：含五元膦-氧螯合环的1，3-二-(2，6-二甲苯基)-4，5-二氢咪唑基1-苯亚甲基--一氯合钌(46)、含六元柔性膦-氧螯合环的[1，3-二-(2，6-二甲苯基)-4，5-二氢咪唑基1-苯亚甲基--一氯合钌(47)及含六元刚性膦-氧螯合环的[1，3-二-(2，6-二甲苯基)-4，5-二氢咪唑基]-苯亚甲基--一氯合钌(48)。X射线单晶衍射分析证明，配合物46、47都为变形的四方锥构型，膦-氧与钌形成螯合配位，其中苯亚甲基与钌的配位得以加强。

The famciclovir was synthesized from purine by a series of steps by Acylation, Decarboxylation, Reduction ,and so on; Derivatives of these intermediates is described from the 6-chloro- 9H- purin-2-amine as raw materials in different conditions when the iodine and bromide were synthesized with the addition of two intermediate 6-bromo-9H-purin-2-amine and 6-iodo-9H-purin-2-amine; There is elaborated from the main part of a acetophenone, urineaminohydrochloride, phenylhydrazine, ethyl acetoacetate as raw material through a series of reactions to synthetic 3-phenyl-4-formylphenyl pyrazole and 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-aldehyde two pyrazole aldehyde, and then with 2-amino-6-chlorine-9-(2-methicillin-oxo-co-methyl-4-yl) purine reaction of the two new pyrazole purine Schiff bases.

本论文主是采用以鸟嘌呤为原料，经过一系列的酰基化，脱羧，还原等反应作用下最终得到了产物2-氨基-9-(4-乙酰氧基-3-乙酰氧基甲基丁基)嘌呤；其中的中间体衍生物主要是阐述从以2-氨基-6-氯鸟嘌呤为原料通过在不同的条件下进行溴代与碘代分别合成了另外两种中间体2-氨基-6-溴鸟嘌呤及2-氨基-6-碘鸟嘌呤；还有一部分主要是阐述从以苯乙酮，盐酸氨基脲，苯肼，乙酰乙酸乙酯为原料通过一系列的反应先合成3-苯基-4-醛基吡唑及5-氯-3-甲基-1-苯基-1H-吡唑-4-甲醛这两个吡唑醛，然后再与2-氨基-6-氯-9-(2-甲氧羰基丁酸甲酯-4-基)嘌呤反应得到了两个新型的吡唑嘌呤席夫碱

In the third step, when the ratio of racemic ester to benzenesulfonyl chloride to triethylamine to catalyst 4-DMAP is 1:1:1:0.1 in 10℃, the yield is 82.9% and high purity is obtained by crystallisation.

在第三步磺酰化反应中，得到合成消旋2-苯磺酸基-2(2-氯苯基)乙酸甲酯的较佳反应条件为邻氯扁桃酸甲酯：苯磺酰氯：三乙胺=1：1：1，催化剂4-DMAP用量为摩尔反应物的10%，反应温度为10℃，收率为82.9%，同时用结晶方法获得高纯度的产物。

A method used to simutaniously analyze the residues of herbicides 2, 4-dichlorophenoxyacetic acid (2,4-D), 2-(2,4-dichiorophenoxy) propanoic acid (2,4-DP) and 2,4-dichiorophenoxybutyric acid (2,4-DB) in garlic was developed in our study.

本研究建立了一种应用基质固相分散－高效液相色谱法，同时测定大蒜中2，4-二氯苯氧乙酸、2，4-二氯苯氧丙酸及2，4-二氯苯氧丁酸等3种2，4-D类除草剂残留的方法。

The split between the two groups can hardly be papered over.

这两个团体间的分歧难以掩饰。

This approach not only encourages a greater number of responses, but minimizes the likelihood of stale groupthink.

这种做法不仅鼓励了更多的反应，而且减少跟风的可能性。