乙酰乙酸

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。

Major procurement of goods: a three-chlorosilanes, dichloromethane, AE activity ester, 3-iodine Silane, special acid, pentyl chloride, triethylamine, thiadiazole, tetrazolylazo acid, 2 - Acetamide, tetrahydrofuran, the four-guanidine, isopropanol, five phosphorus trichloride, sodium vary bitter, acid, sodium phenylacetate, 6-2 silicon n-amine, Ethylacetoacetate , Methyl isobutyl ketone, potassium dihydrogen phosphate, aluminium oxide, DL methionine, N, N-dimethylaniline, NN-diethyl aniline, 4 sodium EDTA, Anhydrous sodium sulfate, ammonium sulfate, potassium sulfate, sodium acetate, sodium carbonate, DMC, formic acid, sodium chloride medicinal, oxalate, protopine, acetone, alcohol, acetic acid, vinegar Ethyl, butyl acetate, methanol, ethanol (anhydrous, industrial, medicinal), formaldehyde, Ye Jian (30%), hydrochloride (industrial-grade, refined grade, reagent level), sulfate (98%), Ammonia, calcium carbonate, chlorine dioxide, 6 - APA ,7-ACA ,7-ADCA ,7-ANCA, sulbactam, ceftazidime activity ester, Deng salt (hydroxymethyl-K, acid precursors Potassium, sodium dihydrogen methyl), resin, the enzyme, water treatment agent, Xiao Mo agent, demulsifier, flocculants, activated carbon, all kinds of medicinal materials, All kinds of additives

三甲基一氯硅烷、二氯甲烷、AE活性酯、三甲基碘硅烷、特戊酸、特戊酰氯、三乙胺、噻二唑、四氮唑乙酸、二甲基乙酰胺、四氢呋喃、四甲基胍、异丙醇、五氯化磷、异辛酸钠、苯乙酸、苯乙酸钠、六甲基二硅胺烷、乙酰乙酸乙酯、甲基异丁酮、磷酸二氢钾、三氧化二铝、DL蛋氨酸、N，N-二甲基苯胺、NN-二乙基苯胺、乙二胺四乙酸四钠、无水硫酸钠、硫酸铵、硫酸钾、醋酸钠、碳酸钠、碳酸二甲酯、甲酸、药用氯化钠、草酸、片碱、丙酮、正丁醇、冰醋酸、醋酸乙酯、醋酸丁酯、甲醇、乙醇、甲醛、液碱（30％）、盐酸（工业级、精制级、试剂级）、硫酸（98％）、氨水、碳酸钙、二氧化氯、6－APA、7－ACA、7－ADCA 、7－ANCA、舒巴坦、头孢他啶活性酯、邓盐(羟甲基钾、前体酸钾、二氢甲基钠)、树脂、生物酶、水处理剂、消沫剂、破乳剂、絮凝剂、活性碳、各种药用辅料、各种添加剂

Mission:"equality and mutual benefit, reputation first, unity and cooperation and friendship between the long-term" supply products: ethylenediamine; diethylamide; triethylamine; Diethylenetriamine; three ethylene diamine; three ethylene amines 40; 40 Five ethylene amines; five ethylene amines 6; caprolactam; DMF; allyl amine; N, N dimethylaniline; propylamine; are butylamine; are TOA; 3 Poly Cyanamide; 1,2 c diamine; ethanolamine; diethanolamine, triethanolamine; potassium iodide, potassium hydroxide, potassium permanganate, toluene, xylene, toluene of chlorine ; Acetone, butanone; acetylacetone; ethyl acetate, butyl acetate; Y-butyrolactone; DMC; acetyl of methyl acetate; Sanfu acetyl acid; Sanfu acetyl B Ethyl; methanol, ethanol, isopropanol; propylene glycol; glycerol; propargyl alcohol; 1.3 propylene glycol; xylitol; acetic acid; have acid; mercaptoacetic acid; vary Bitterness; adipic acid; trifluoroacetic acid; oxalic acid, the amino acid; o-amygdalin acid; DL-Acid; anhydrous piperazine; six non-piperazine, furfural, castor oil, ethylene Aldehyde; glutaraldehyde, multi-POM; isopropyl ether; anisole; tetrahydropyrrole; pure pyridine; 1.2 dichloroethane; methylene chloride, chloroform, carbon tetrachloride; hydrazine hydrate; Nonylphenol;-m-cresol; Se phenol; phenol; the tert-butyl phenol; Titanium Dioxide; iron; full Tangfen; Bisphenol A; azo two different nitrile; sodium azide; sodium carbonate ; Sodium chloride; iron oxide; cuprous chloride; thionyl chloride; D4; sodium bicarbonate; ammonia, potassium chloride; anhydrous sodium sulphite; ammonium persulfate; glycol Dingmi; B Glycol ether; calcium chloride; cyclohexanone; cyclohexane, methyl tertiary butyl ether, potassium carbonate, ferric chloride, potassium nitrate; Linsuansanna; zinc oxide; sodium nitrite; antimony oxide; Tartrate; OP-10; TX-10; tablets base; AES; sodium benzoate, sodium citrate; partial sodium silicate, sodium perborate, a sodium carbonate, sodium benzene; Asia sodium chlorate; Wuluo Care products; urea; hydrochloric acid, sulfuric acid, lactic acid; amino acid, hydrogen peroxide, ammonium bicarbonate

公司宗旨："平等互利，信誉至上，团结合作，友谊长久"乙二胺；二乙胺；三乙胺；二乙烯三胺；三乙烯二胺；三乙烯四胺；四乙烯五胺；五乙烯六胺；己内酰胺；二甲基甲酰胺；烯丙基胺；N，N二甲基苯胺；正丙胺；正丁胺；正辛胺；三聚氰胺；1，2丙二胺；一乙醇胺；二乙醇胺；三乙醇胺；碘化钾；氢氧化钾；高锰酸钾；甲苯；二甲苯；对氯甲苯；丙酮；丁酮；乙酰丙酮；醋酸乙酯；醋酸丁酯；Y-丁内酯；碳酸二甲酯；乙酰乙酸甲酯；三伏乙酰乙酸；三伏乙酰乙酸乙酯；甲醇；无水乙醇；异丙醇；丙二醇；丙三醇；丙炔醇；1.3丙二醇；木糖醇；冰醋酸；己醛酸；巯基乙酸；异辛酸；己二酸；三氟乙酸；乙二酸；对氨基苯乙酸；邻氯苦杏仁酸；DL-扁桃酸；无水哌嗪；六无哌嗪；糠醛；蓖麻油；乙二醛；戊二醛；多聚甲醛；异丙醚；苯甲醚；四氢吡咯；纯吡啶；1.2二氯乙烷；二氯甲烷；三氯甲烷；四氯化碳；水合肼；壬基酚；纯间甲酚；硒酚；苯酚；对叔丁基苯酚；钛白粉；铁粉；全糖粉；双酚A；偶氮二异丁腈；叠氮化钠；碳酸钠；氯化钠；三氧化二铁；氯化亚铜；氯化亚砜；D4；碳酸氢钠；氨水；氯化钾；无水亚硫酸钠；过硫酸铵；乙二醇丁醚；乙二醇乙醚；氯化钙；环己酮；环己烷；甲基叔丁基醚；碳酸钾；三氯化铁；硝酸钾；磷酸三钠；氧化锌；亚硝酸钠；氧化锑；酒石酸；OP-10；TX-10；粒碱；AES；苯甲酸钠；柠檬酸钠；偏硅酸钠；过硼酸钠；过碳酸钠；苯磺酸钠；亚氯酸钠；乌洛托品；尿素；盐酸；硫酸；乳酸；氨基磺酸；双氧水；碳酸氢铵

A set of laser monitoring observation system to be used for measure the solubility with a high speed, which is programmed heating apparatus , have designed. The solubility of 1,2-cyclohexanediol were measured in water, methyl acetate, acetic ester, propyl acetate, butyl acetate, methyl acrylate, ethyl acrylate, acetoacetic ester at different temperature.

另外，还建立了一套带激光监视系统，可以控制升温速率的溶解度测定实验装置，测定了反式-1，2-环己二醇在水、乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、乙酰乙酸乙酯、丙烯酸甲酯、丙烯酸乙酯和甲基丙基酮等9个二元体系中的溶解度。

objective to determine the contents of residual acetone in acetoacetic ester,the raw material for the synthesis of edaravone, by gas chromatography.methods sample solution was injected on a gdx column (0.18 mm～0.25 mm) with nitrogen as the carrier gas.the residue was calculated by the external standard method.results the linearity was good over the range of 25 μg/ml～400 μg/ml,with the correlation coefficient of acetone being 0.996 and the average recovery 96.8%.conclusions the method was proved to be simple,rapid,practical and highly sensitive.it is an efficient method for the quality control of acetoacetic ester.

摘要］ 目的：用气相色谱法测定依达拉奉合成起始原料乙酰乙酸乙酯中丙酮的残留量。方法：采用固定相为二乙烯苯乙基乙烯苯型高分子多孔小球（直径为0.18 mm～0.25 mm），氮气为载气，用外标法测定乙酰乙酸乙酯中残留丙酮的含量。结果：该方法在丙酮浓度范围在25 μg/ml～400 μg/ml内呈良好的线性关系，响应曲线相关系数为0.996，平均回收率为96.8%。结论：本法简便，快速、实用，灵敏度高，可有效地用于乙酰乙酸乙酯的质量控制。

Objective To determine the contents of residual acetone in acetoacetic ester,the raw material for the synthesis of Edaravone, by gas chromatography.Methods Sample solution was injected on a GDX column (0.18 mm～0.25 mm) with nitrogen as the carrier gas.The residue was calculated by the external standard method.

摘要］ 目的：用气相色谱法测定依达拉奉合成起始原料乙酰乙酸乙酯中丙酮的残留量方法：采用固定相二乙烯苯乙基乙烯苯型高分子孔小球（直径为0.18 mm～0.25 mm），氮气为载气，用外标法测定乙酰乙酸乙酯中残留丙酮的含量。

Mission:"equality and mutual benefit, reputation first, unity and cooperation and friendship between the long-term" supply products: ethylenediamine; diethylamide; triethylamine; Diethylenetriamine; three ethylene diamine; three ethylene amines 40; 40 Five ethylene amines; five ethylene amines 6; caprolactam; DMF; allyl amine; N, N dimethylaniline; propylamine; are butylamine; are TOA; 3 Poly Cyanamide; 1,2 c diamine; ethanolamine; diethanolamine, triethanolamine; potassium iodide, potassium hydroxide, potassium permanganate, toluene, xylene, toluene of chlorine ; Acetone, butanone; acetylacetone; ethyl acetate, butyl acetate; Y-butyrolactone; DMC; acetyl of methyl acetate; Sanfu acetyl acid; Sanfu acetyl B Ethyl; methanol, ethanol, isopropanol; propylene glycol; glycerol; propargyl alcohol; 1.3 propylene glycol; xylitol; acetic acid; have acid; mercaptoacetic acid; vary Bitterness; adipic acid; trifluoroacetic acid; oxalic acid, the amino acid; o-amygdalin acid; DL-Acid; anhydrous piperazine; six non-piperazine, furfural, castor oil, ethylene Aldehyde; glutaraldehyde, multi-POM; isopropyl ether; anisole; tetrahydropyrrole; pure pyridine; 1.2 dichloroethane; methylene chloride, chloroform, carbon tetrachloride; hydrazine hydrate; Nonylphenol;-m-cresol; Se phenol; phenol; the tert-butyl phenol; Titanium Dioxide; iron; full Tangfen; Bisphenol A; azo two different nitrile; sodium azide; sodium carbonate ; Sodium chloride; iron oxide; cuprous chloride; thionyl chloride; D4; sodium bicarbonate; ammonia, potassium chloride; anhydrous sodium sulphite; ammonium persulfate; glycol Dingmi; B Glycol ether; calcium chloride; cyclohexanone; cyclohexane, methyl tertiary butyl ether, potassium carbonate, ferric chloride, potassium nitrate; Linsuansanna; zinc oxide; sodium nitrite; antimony oxide; Tartrate; OP-10; TX-10; tablets base; AES; sodium benzoate, sodium citrate; partial sodium silicate, sodium perborate, a sodium carbonate, sodium benzene; Asia sodium chlorate; Wuluo Care products; urea; hydrochloric acid, sulfuric acid, lactic acid; amino acid, hydrogen peroxide, ammonium bicarbonate

公司宗旨：&平等互利，信誉至上，团结合作，友谊长久&乙二胺；二乙胺；三乙胺；二乙烯三胺；三乙烯二胺；三乙烯四胺；四乙烯五胺；五乙烯六胺；己内酰胺；二甲基甲酰胺；烯丙基胺；N，N二甲基苯胺；正丙胺；正丁胺；正辛胺；三聚氰胺；1，2丙二胺；一乙醇胺；二乙醇胺；三乙醇胺；碘化钾；氢氧化钾；高锰酸钾；甲苯；二甲苯；对氯甲苯；丙酮；丁酮；乙酰丙酮；醋酸乙酯；醋酸丁酯；Y-丁内酯；碳酸二甲酯；乙酰乙酸甲酯；三伏乙酰乙酸；三伏乙酰乙酸乙酯；甲醇；无水乙醇；异丙醇；丙二醇；丙三醇；丙炔醇；1.3丙二醇；木糖醇；冰醋酸；己醛酸；巯基乙酸；异辛酸；己二酸；三氟乙酸；乙二酸；对氨基苯乙酸；邻氯苦杏仁酸；DL-扁桃酸；无水哌嗪；六无哌嗪；糠醛；蓖麻油；乙二醛；戊二醛；多聚甲醛；异丙醚；苯甲醚；四氢吡咯；纯吡啶；1.2二氯乙烷；二氯甲烷；三氯甲烷；四氯化碳；水合肼；壬基酚；纯间甲酚；硒酚；苯酚；对叔丁基苯酚；钛白粉；铁粉；全糖粉；双酚A；偶氮二异丁腈；叠氮化钠；碳酸钠；氯化钠；三氧化二铁；氯化亚铜；氯化亚砜；D4；碳酸氢钠；氨水；氯化钾；无水亚硫酸钠；过硫酸铵；乙二醇丁醚；乙二醇乙醚；氯化钙；环己酮；环己烷；甲基叔丁基醚；碳酸钾；三氯化铁；硝酸钾；磷酸三钠；氧化锌；亚硝酸钠；氧化锑；酒石酸；OP-10；TX-10；粒碱；AES；苯甲酸钠；柠檬酸钠；偏硅酸钠；过硼酸钠；过碳酸钠；苯磺酸钠；亚氯酸钠；乌洛托品；尿素；盐酸；硫酸；乳酸；氨基磺酸；双氧水；碳酸氢铵

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。

Base played a crucial role in this reaction: in the Pd2/L1 catalyzed α-arylation of ethyl malonate, K3PO4 is the base of choice; in the α-arylation of ethyl acetoacetate, K2CO3 is the most effective base.

在这类催化反应中，碱的选择具有重要的影响：以K3PO4为碱， Pd2/L1催化体系在丙二酸二乙酯的α-芳基化中，富电子溴代芳烃显示较好的活性； Pd2/L1催化的乙酰乙酸乙酯α-芳基化时，以 K2CO3为碱，催化体系显示较好的活性，这个催化体系可控制反应得到α-芳基乙酰乙酸乙酯，而不是脱乙酰基的产物。

Base played a crucial role in this reaction: in the Pd2/L1 catalyzed α-arylation of ethy malonate, K3PO4 is the base of choice; in the α-arylation of ethyl acetoacetate, K2CO3 is the most effectiv base.

在这类催化反应中，碱的选择具有重要的影响：以K3PO4为碱，Pd2/L1催化体系在丙二酸二乙酯的α-芳基化中，富电子溴代芳烃显示较好的活性；Pd2/L1催化的乙酰乙酸乙酯α-芳基化时，以K2CO3为碱，催化体系显示较好的活性，这个催化体系可控制反应得到α-芳基乙酰乙酸乙酯，而不是脱乙酰基的产物。

I didn't watch TV last night, because it .

昨晚我没有看电视，因为电视机坏了。

Since this year, in a lot of villages of Beijing, TV of elevator liquid crystal was removed.

今年以来，在北京的很多小区里，电梯液晶电视被撤了下来。