乙酰乙酸

Methods Protein in blood and urine was precipitated directly by acetonitrile with acetanilide was used as the internal standard using Agilent Zorbax SB-Aq column (250 mm×4.6 mm, 5 μm). The mixed solvents of water (triethylamine 0.12%, acetic acid 0.12%) and acetonitrile were used as the mobile phase to separate cephalosporins using gradient elution method at 1 mL/min and 254 nm.

以乙酰苯胺为内标，血液和尿液用乙腈直接沉淀蛋白，采用Agilent Zorbax SB-Aq(250 mm×4.6 mm， 5 μm)色谱柱，流动相选用水（含0.12%三乙胺和0.12%乙酸）和乙腈的混合溶剂梯度洗脱，流速1 mL/min，检测波长254 nm。

Six derivatives of 4-phenyl-3-phenoloxymethyl-5-mercapto-1,2,4-triazlyole were synthesized from phenoloxyacetyl hydrazide by two-steps reaction under microwave irradiation, then reacted with 2-chloroacetic acid to give six novel derivatives of 2-(3-phenoxymethyl-4-phenyl-[1,2,4]triazole-5-thio)-acetic acid.

在微波辐射条件下，芳氧乙酰肼经两步反应制得4-苯基－3-芳氧甲基－1，2，4-三唑－5-硫酮衍生物，再与氯乙酸反应得到6种尚未见文献报道的2-（3-芳氧甲基－4-苯基－1，2，4-三唑－5-硫基）乙酸衍生物。

Project Background and Conditions: The company started research new chemical products in 1998. After two years of efforts, a series of pharmaceutical intermediate sulfathiazole leave instructions, including : 3- methyl sulfathiazole leave instructions, 2- sulfathiazole leave instructions ethanoic acid, 2- acetyl sulfathiazole leave instructions, 2-thiofuran amino ethane ,2-thiofuran acetic, 3,4,5- tighter nitrobenzene have been successfully developed. 2-thiofuran amino ethane are the precursors raw materials of series antibiotic analgesic.

二、项目建设背景及条件：1998年公司开始研究开发高新精细化工产品，经过两年的努力，已成功研制出噻吩系列医药中间体，包括：3-甲基噻吩、2-噻吩乙酸、2-乙酰噻吩、2-噻吩乙胺、2-噻吩乙醇、3，4，5-三氯硝基苯等。2-噻吩乙胺系列噻吩产品使用于血小板及血栓有关的心脏血管病及消炎镇痛等如氯吡格雷、兴孢噻吩钠、兴孢西丁、噻吩洛酸等十几种新药的前体原料，是国家政策鼓励发展和有自主知识产权的项目。

Results show that, by using thionyl chloride and N,N-dimethyl formamide as chlorinating reagent and dichloromethane as solvent and taking -15℃ as reaction temperature, Z-iomer crystals with pale white color and stable to temperature can be obtained with an overall yield of 70%.

以2-（2-氨基噻唑－4-基）－2-甲氧亚氨基乙酸为原料，经盐酸化、氯代等反应合成了Z-2-（2-氨基噻唑－4-基）－2-甲氧亚氨基乙酰氯盐酸盐；氯代时以用亚硫酰氯和N，N-二甲基甲酰胺的混合物代替五氯化磷作氯化剂，并考察了温度和溶剂对氯代产物中Z-异构体和E-异构体收率的影响。

The results showed that there were 8 kinds of aliphatic, 5 kinds of esters, 2 kinds of aldehydes, 2 kinds of nitrogen sulfur heterocyclic rings and one kind of hydrocarbon, alcoholics, ketone, lactones respectively in the analyzed 21 kinds of aroma components, and the content of furfural,β-methyl valeric acid, palmitic acid, nicotine, neohytadiene were higher, next were acetyl ethyl propionate, caleric acid, phenyl ethyl acetate, hydroxylic diethyl succinate.

结果表明，在分析出的21种香气成分中，分别有脂肪酸类8种，酯类5种，醛类2种，氮硫杂环类2种，烃类、醇类、酮类、内酯类各l种，其中相对含量较高的物质成分是糠醛、β-甲基戊酸、十六碳酸、烟碱、新植二烯，其次是乙酰丙酸乙酯、异戊酸、苯乙酸乙酯、羟基丁二酸二乙酯等。

Chapter 2 has analysized the conversly synthetic means of solanesol and designed novelly synthetic routes of solanesol and key intermediate Chapter 3 has summarized the preparation of trans-3-methyl-4-hydroxy (bromo-2-butenyl oxy methyl benzene In chapter 4 ,a novel technology of important intermediate(all trans-8-bromo geranyl acetate),which is suitable for industrial procedure , was found .meanwhile,an another new way has been invented ,of which the key intermediate (all trans-8-hydroxy geranyl acetate) has been produced.

第二部分分析了茄尼醇的逆合成方法，设计了一条适合于合成茄尼醇的合成路线及其重要中间体的合成路线。第三部分研究了重要中间体[Trans-3-甲基-4-羟基-2-丁烯基乙酰基(苄基，2，3-二氢吡喃基)醚]的合成新方法，找到了一条适合于工业化生产的制备反式-3-甲基-4-羟基-2-丁烯基苄基醚的新方法。第四部分研究了重要中间体[-3，7-二甲基-8-羟基-2，6-辛二烯-1-醇乙酸酯、-3，7-二甲基-8-溴-2，6-辛二烯-1-醇乙酸酯]的合成新方法，找到了一条适合于工业化生产的制备它们的新方法；同时研究了一条制备-3，7-二甲基-8-羟基-2，6-辛二烯-1-醇乙酸酯的另一新方法。

The first synthetic route uses 1,2,4-trimethoxybenzene and chloroacetonitrile in forming 2,4,5-trimethoxy-a-chlor-acetophenone under the anhydrous condition, then the intermediate condensates with papaverine forming the core pyrro[2,l-a]isoquinoline, followed by formation and lactonization to form the lactone ring. The second synthetic route uses prepared aldehyde with prepared ethyl nitroacetate by Knoevenagel condensation to obtain 2-Nitro-3-(2,4,5-tris-methoxy-phenyl)-acrylic acid ethyl ester and 2-Nitro-3-(2,4,5-tris-benzyloxy -phenyl)-acrylic acid ethyl ester etal intermediates. The lamellarin skeleton could arise from condensation of the papaverine and these intermediates by Michael reaction, the ester group is provided for subsequent lactonization. The third synthetic route uses coumarin or indan-l,3-dione derivatives and papaverine to form lamellarin under basic conditions.

第一条路线首先从1，2，4-三甲氧基苯出发与卤乙腈作用合成卤代芳酮中间体，然后与罂粟碱反应合成开链片螺素，最后经乙酰化、去保护、成内酯环得到片螺素；第二条路线由制备的芳醛和制备的硝基乙酸乙酯经缩合得到2-硝基-3-芳基丙烯酸乙酯，然后由该中间体与罂粟碱反应，在完成关环的同时也引入酯基，最后去保护、成内酯环得到片螺素；第三条路线是由香豆素或茚二酮出发，经溴代后的中间体与罂粟碱反应，得到片螺素的基本框架。

Results: Diacetyl monoxime solution of acetic acid and to without acetic acid DMA color liquid, transparent tube and the Brown tube of absorbance determination, 30 min to put average drop of 6.80%, 1.30% and 1.44%, 0.98%; 60 min put average drop 19.8%, 1.92% and

结果：二乙酰一肟乙酸溶液与无乙酸的DMA显色液，其透明管与遮光管测定的吸光度，放置30 min平均下降了6.80%、1.30%与1.44%、0.98%；放置60 min平均下降了19.8%、1.92%与2.49%、1.60%。

The similar nicotinoyltrifluoroacetones are synthesized from acetylpyridine and ethyl trifluoroacetate through Claisen reaction.The influnences of alcoholic natrium,reaction temperature and solvent on reaction yield is studied.The subliming method is improved.

本文以乙酰吡啶和三氟乙酸乙酯为主要原料，利用克莱森酯缩合反应，合成了三种相似结构的吡啶甲酰三氟丙酮化合物，考察了碱性试剂醇钠、反应温度和溶剂等因素对反应产率的影响，改进了纯化产物的方法。

Treatment of sucrose alkyl 4,6-orthoacetate hexaacetates I with water or alcohol in the presence of an acid catalyst afforded derivatives of sucrose acetates by selectively blocking specific hydroxyl group in sucrose and acetyl migration.

4，6-原乙酸蔗糖六乙酸酯在酸催化下水解和醇解，选择性地保护了蔗糖分子中的某些羟基，并通过乙酰基由C~4→C~6迁移的异构化反应合成了一系列蔗糖乙酸酯。

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。