乙酰氯

The optimum reaction conditions are as follows: diphenylmethanethiol : methyl chloroacetate is 1:1.5, and the reaction carried out at 100℃ for 4 h, 2- acetamide can be carried out in the room temperature for 20 h, the yield of 2- acetamide was 76%, hydrogen dioxide: 2- acetamide is 1:1, and the reaction carried out at 60℃ for 3 h, the yield of modafinil was 79%, the total yield of reaction can be reached 48%.

研究表明，采用氯乙酸甲酯作为醚化试剂，反应时间4h，反应温度100℃，二苯甲硫醇：氯乙酸甲酯=1：1.5，室温下氨解反应20h，二苯甲硫乙酰胺收率76%；采用过氧化氢作为氧化试剂，反应时间3h，反应温度60℃，过氧化氢：二苯甲硫乙酰胺=1：l，莫达非尼收率79%，反应总收率可达48%。

In this paper, acetanilide used as start material was chlorosulfonated, then reacted with alkylamines with different length of carbon chain to prepare 4 p-acetylaminophenylsulfonylalkylamine.

本文以乙酰苯胺为起始原料，经氯磺化后分别和不同碳链的正烷基胺反应制得4种不同碳链长度的对乙酰氨基苯磺酰烷基胺，将其水解后制得了对氨基苯磺酰正丁胺、对氨基苯磺酰正辛胺、对氨基苯磺酰正十二胺和对氨基苯磺酰正十八胺。

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。

A series of p-toluene sulfonylamido acetacylhydrazone derivatives were synthesized from p-toluenesulfonyl chloride which reacted with glycine to get the intermediate p-toluene sulfonylamido glycine, then through the esterification, hydrazinolysis to afford another intermediate p-toluene sulfonylamido acethydrazide, which condensed with different aldehydes to obtain the target compounds that were characterized by IR, 1H NMR, 13C NMR spectra and elemental analysis.

魏太保 ；冷艳丽；王永成；张建辉；张有明*摘要：以对甲苯磺酰氯为原料，通过与氨基乙酸反应得到中间体对甲苯磺酰氨基乙酸，再经酯化、肼解得到对甲苯磺酰氨基乙酰肼，然后与相应的醛缩合得一系列对甲苯磺酰胺基乙酰腙类化合物。其结构经元素分析， IR， 1H NMR和13C NMR确证。

Firstly, 3-ethylthiobutanal was prepared from crotonaldehyde reacting with ethanehiol in triethylamine with high yield. Secondly, methyl acetoacetate was converted to 6-ethylthiohept-3-en-2-one by three steps via hydrolysis, condensation with 3-ethyltio-butanal and dehydration, then 6-ethylthiohept-3-en-2-one was cycloco ndensed with dimethyl malonate by Michael addition and Claisen condensation, followed by saponification and decarboxylation to give the intermediate of 5-(2-ethylthiopropyl)-cyclohexane-1,3-dione.

首先，以巴豆醛与乙硫醇为原料，在三乙胺的催化作用下高收率制得3-乙硫基丁醛；然后从乙酰乙酸甲酯出发，通过碱水解、与3-乙硫基丁醛缩合、脱水三步反应合成6-乙硫基-3-烯-2-庚酮，接着6-乙硫基-3-烯-2-庚酮与丙二酸二甲酯通过Michael加成和Claisen缩合成环，再通过皂化和脱羧反应生成中间体5-[2-丙基]-1，3-环己二酮；再与丙酸酐反应丙酰化，最后与0-3-氯-2-丙烯基羟胺肟化，得到目标化合物烯草酮。

Through condensing o-aminobenzoic acid, ethyl oxalyl chloride and ethylenediamine(or 1,2-propylenediamine), two new ligands N-benzoato-N′-(2- aminoethyl)oxamido(H3oxbe) and N-benzoato-N-(2-amino-2-methylethyl)oxamido(H3oxbt) have been synthesized. Their mononuclear complexes Na·1.5H2O and Na·1.5H2O have also been obtained.

2以邻氨基苯甲酸、草酸乙酯酰氯和乙二胺(或1，2-丙二胺)缩合制得了两种具有不对称草酰胺结构配体N-(2-苯甲酰基)-N&-(2-氨乙基)草酰胺(H3oxbe)和N-(2-苯甲酰基)-N&-(2-氨丙基)草酰胺(H3oxbt)，并得到了它们的单核配合物：Na·1.5H2O和Na·1.5H2O。

As a key step of the synthesis, the Friedel-crafts acylation was researched. And the optimal operation variables were determined through orthogonal experiment: when 0.lmol acetanilide, 0.26mol aluminum chloride, 0.12mol propionyl chloride and 200ml carbon disulfide are introduced, and the reaction time is 5 hour, the yield can be up to 57.3%. The solid super acid catalyst was preliminary studied. Four solid super acid catalysts were prepared to take the place of aluminum chloride, and it was indicated that AlCl3 acidic resin can better catalyze the Friedel-Crafts reaction of acetanilide.

对合成路线中的Friedel-Crafts酰基化反应进行了研究，运用正交实验设计确定了最佳工艺条件：当乙酰苯胺用量为0.1mol时，AlCl_3用量为0.26mol、丙酰氯用量为0.12mol、溶剂用量为200ml、反应时间为5h，产率可达到57.3％；对于固体超强酸催化剂进行了初步研究，合成了四种催化剂，其中负载AlCl_3强酸性树脂对于乙酰苯胺的Friedel-Crafts酰基化具有一定的催化活性。

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。

Cellulose benzoate,the degree of substitution of which was calculated from the content of C determined by element analysis,was prepared from microcrystalline celluloseand benzoyl chloride under heterogeneous condition and characterized by FT-IR and~1H-NMR.

研究了微晶纤维素和苯甲酰氯在多相条件下合成制备纤维素苯甲酸酯的反应，通过元素分析所得碳的质量百分含量计算了产物的取代度，并系统研究了吡啶与N，N-二甲基乙酰胺或与三乙胺混合反应溶剂、苯甲酰氯与纤维素羟基的摩尔比r、反应温度和反应时间对D S的影响，用FT-IR和1H-NM R对产物进行了表征。

Piperidinecarboxylic acid is used as the raw material and acetic acid as the acylating agent, followed by the addition of some acetic anhydride in the later stage to get an important organic intermediate n-acetylpiperidine-4 carboxylic acid in the yield of 92%. Toluene is used as the solvent instead of sulfinyl chloride in the acyl chlorination to produce n-acetylpiperidine-4-carbonyl chloride with the yield of 97%.

以4-哌啶甲酸为原料、醋酸为酰化剂，后期加入少量醋酸酐反应得到中间体N-乙酰基哌啶－4-甲酸，收率92%；在甲苯溶剂中进行酰氯化得目标产物N-乙酰基哌啶－4-甲酰氯，收率97%。

According to the clear water experiment, aeration performance of the new equipment is good with high total oxygen transfer coefficient and oxygen utilization ratio.

曝气设备的动力效率在叶轮转速为120rpm～150rpm时取得最大值，此时氧利用率和充氧能力也具有较高值。

The environmental stability of that world - including its crushing pressures and icy darkness - means that some of its most famous inhabitants have survived for eons as evolutionary throwbacks, their bodies undergoing little change.

稳定的海底环境─包括能把人压扁的压力和冰冷的黑暗─意谓海底某些最知名的栖居生物已以演化返祖的样态活了万世，形体几无变化。