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乙酰甲基

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Experimental solubilities of terephthalic acid dissolved in N,N-dimethyl propionamide, N,N-diethyl propionamide and N,N-diethyl acetamide were determined in the temperature range of

测定了303.2~363.2K温度范围内,对苯二甲酸在N,N-二甲基丙酰胺、N,N-二乙基丙酰胺和N,N-二乙基乙酰胺中的溶解度。

Ophenyl phenol,ophenyl phenol sodium salt tetrahydrate,7ADCA,2ethyl phenyl hydrazine hydrochloride,2,3dihydrofuran,7ethyl3(2hydroxy ethyl)indole,methyl ester of etodolac; 1,8diethyl1,3,4,9tetrahydropyrano[3.4b] indole1acetic acid methyl ester,5chloro2methoxy benzoic acid,4(2aminoethyl)benzene sulfonamide,5cyano phthalide,phthalhydrazide,9thioxanthenone,n[(1,4benzodioxane2yl)carboxyl]piperazine HCL,2chloro4amino6,7dimethoxyquinazoline,2chloro benzimidazole,1(4fluorobenzyl)2chlorobenzimidazole,2methylthio4pyrimidone,5amino4imidazole carboxamide HCL,6chloro2hexanone,11oxo6.11hydrodibenzothiepin,6,11dihydrodibenzooxepin11one,10,11dihydrodibenzocyclohepten5one;dibenzosuberone,dibenzo cyclohepten5one;dibenzosuberenone,3,5dihydroxy benzoic acid,3,5dihydroxy benzyl alcohol,2mercapto benzimidazole,3,4dihydroxy benzaldehyde,3,4dihydroxy benzonitrile,2amino5chloro benzonitrile,2(4chlorophenoxy)ethyl chloride,2(4chloro phenoxy)tert,butane,ditrimethylol propane;DTMP,2,2bis(4hydroxyphenyl)butane; bisphenol B,1,1'bis(4hydroxyphenyl)cyclohexane;bisphenol Z,tetrabromobisphenolS,3,5ditertbutyl salicylic acid,3,4,5trihydroxy benzoic acid stearyl ester,1,2,4trimethoxybenzene.

华业公司产品:邻苯基苯酚,邻苯基苯酚钠盐,7氨基3去乙酰氧基头孢烷酸,邻乙基苯肼盐酸盐,2,3二氢呋喃,7乙基色氨醇,依托度酸甲酯,5氯2甲氧基苯甲酸,4(2氨乙基)苯磺酰胺,5氰基苯酞,双酮酞嗪,9噻吨酮,N〔(1,4苯并二恶烷2基)羰基〕哌嗪盐酸盐,2氯4氨基6,7一二甲氧基喹唑啉,2氯苯并咪唑,1(4氟苄基)2氯苯并咪唑,2甲硫基4嘧啶酮,5氨基咪唑4 甲酰胺盐酸盐,6氯2已酮,11氧6.11二氢苯并〔b.c〕虑平,11氧代6,11二氢二苯并氧杂卓,10,11二氢二苯并环庚烯5酮,二苯并环庚烯5酮,3,5二羟基苯甲酸,3,5二羟基苯甲醇,2巯基苯并咪唑,3,4二羟基苯甲醛,3,4二羟基苯腈,2氨基5氯苯腈,2(4氯苯氧基)1氯乙烷,2(4氯苯氧基)叔丁烷,双丙烷,2,2二(4羟基苯基)丁烷;双酚B,1,1'双(4羟基苯基)环己烷;双酚Z,2[3,5二溴4(2,3二溴丙氧基)]苯砜,3,5二叔丁基水杨酸,3,4,5三羟基苯甲酸十八烷基脂,1,2,4三甲基氧基苯。

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。

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。

The analogs of piracetum with the core of demethylclausenamide(III-4 and III-5) were prepared by condensation of demethylclausenamide with ethyl bromoacetate and hydrolysis or aminolysis there after.

3在兰培工作的基础上,选用O-乙酰-R--扁桃酸为拆分剂,成功的拆分了表黄皮酰胺前体5--4-苯基-1-甲基吡咯烷酮(Ⅱ-1),和Ⅱ-1分别引入3位羟基得到和表黄皮酰胺。

In this thesis,the AM1,MNDO,MINDO/3(mainly AM1)and INDO/S-CI semiempirical MO methods were used toinvestigate the excited-state intramolecular protontransfer reactions of salicylic acid derivatives—salicylic acid,methyl salicylate,salicylaldehyde,o-hydroxyaceto-phenone,salicylamide and 3-hydroxy-picolinamide (6 conformers and 2-3 anion species);2-(2'-hydroxy-5' methylphenyl) benzotriazole(4 conformers),2-(2' hydroxyphenyl) benzimidazole (3 conformers and 3anion species),Bis-2,5-(2-benzoxazolyl)hydroquinone(3 conformers),2-(2'-hydroxyphenyl)benzothiazole(2conformers) and 7-azaindole dimer (2 conformers).Theinvestigations were described as follows.Geometry optimization,relative stability andhydrogen bonding energy First,for sylicylic acid derivative molecules,the AM1,MNDO and MINDO/3 methods were used toinvestigate ground-state geometry optimization,energies,relative stabilities and hydrogen-bondingenergies on the five kinds of the molecules(designing 6 conformers and 2-3 anion species).Comparing with experimental data,the optimizedgeometry,the order of stability,the hydrogen-bonding energies and the distances between O-O in O-H..O hydrogen bonds by AM1 method were in agreementwith the experimental data,however,the C-C bondlengths optimized by MNDO and MINDO/3 were longer,C-O and O-H bond lengths were shorter;for C-N bondlengths,the results opitimized by MNDO method werethe same as those by AM1 method,nevertheless the C-Nbond lengths given by MINDO/3 method were muchshorter.For some sylicylic acid derivatives(e.g.methyl salicylate,salicylamide),the order ofstabilities on the conformers given by MNDO andMINDO/3 methods were not in agreement with theexisting conformers deduced by experimental methods,and the hydrogen bonding energies calculated by MNDO.and MINDO/3 methods were smaller.Second,the studyon the other systems found that the optimizedgeometry of the proton-transfered product with INDOmethod could not be obtained,only could theoptimized geometry of reactant be obtained,and thecalculated hydrogen bonding energies were greater.Many results of calculation indicated that the studyon the excited-state intramolecular proton transferreaction system using AM1 method was suitable andreliable.

本论文用AM1、MNDO、MINDO/3(主要是AM1)和INDO/S-CI半经验分子轨道方法对水杨酸衍生物系列——水杨酸、水杨酸甲酯、水杨醛、O-羟基乙酰苯酮、水杨酰胺和3-羟基吡啶酰胺(6种异构体和2-3种阴离子);2-(2'-羟基-5'-甲基苯基)苯并三〓唑(4种异构体);2-(2'-羟基苯基)苯并咪唑(3种异构体和3种阴离子);2,5-二间氮杂氧茚氢醌(3种异构体);2-(2'-羟基苯基)间〓杂硫茚(2种异构体)和7-〓吲哚二体(2种异构体)的激发态分子内质子转移反应在以下几个方面进行了较系统的理论研究:几何构型优化和相对稳定性及氢键能首先以水杨酸衍生物系列分子为例,用AM1、MNDO和MINDO/3方法考察了5种分子(每种分子设计6种异构体和2-3种阴离子)的基态几何构型优化,能量、相对稳定性和氢键能计算,通过和实验数据进行比较,AM1方法给出的优化几何构型、稳定性次序、氢键能和O—H。。。O氢键的0—0距离与实验数据吻合最好,MNDO和MINDO/3方法优化的C-C键长偏长,C-O键和O-H键长偏短;对于C-N键长,MNDO和AM1优化结果差别不大,而MINDO/3给出了过短的C-N键长,MNDO和MINDO/3方法给出的有些水杨酸衍生物分子(如水杨酸甲酯和水杨酰胺)异构体的稳定性次序和实验上推测的可存在异构体结果不一致,MNDO和MINDO/3方法给出的氢键能偏低,对其他体系的研究发现INDO方法常常不能得到质子转移产物的优化几何构型,只能得到反应物的优化构型,并且估算的氢键能偏高,大量的计算结果表明AM1方法对本论文研究的激发态分子内质子转移反应体系是适宜和可靠的。

Based on broad information collection, author compared and studied on the old synthesis process, and proposed the better process that started from benzyl chloride, then according to the sequence of " synthesis of benzylamine, synthesis of N-benzyl-N--acetamine, synthesis of 2-chloro-5-methylpridine ,2-chloro-5-trichloromethylpyridine,2-chloro-5-trifluropyridine " five steps to get the final product, CTFP.

本文在查阅大量文献资料和对2-氯-5-三氟甲基吡啶合成路线进行分析比较的基础上,提出了较佳合成路线,即以氯化苄为原料,合成的反应步骤为&苄胺&合成、&N-苄基-N--乙酰胺&合成、&2-氯-5-甲基吡啶&合成、&2-氯-5-三氯甲基吡啶&合成、&2-氯-5-三氟甲基吡啶&合成五步。

This thesis consists of four chapters:Chapter 1: Michael addition of chalcones with active methylene compounds such as diethyl malonate, ethyl acetoacetate and nitromethane catalyzed by potassium hydroxide in anhydrous ethanol results Michael adducts in 72-98% yield under ultrasound irradiation in 25-150min.

第一章:研究了超声辐射下,氢氧化钾催化的查耳酮与活泼亚甲基化合物如丙二酸二乙酯、乙酰乙酸乙酯和硝基甲烷的迈克尔反应。

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