二

Is a high-tech private enterprise, located in Laohekou City, Hubei Province, the main products are: 3,4 - dichloro-nitrobenzene; 3,4 - dichloroaniline; 2,4 - dimethyl-nitramine p; 2,4 - dimethylaniline; 2,6 - dimethyl-nitrobenzene; 2,6 - dimethylaniline; 3,5 - dimethyl-nitrobenzene; 3,5 - dimethyl Aniline; acrolein; Glutaraldehyde and other fine chemical products.

老河口联谊化工有限公司为一家高科技民营企业，位于湖北省老河口市，主要产品有：3，4-二氯硝基苯；3，4-二氯苯胺；2，4-二甲基硝基苯；2，4-二甲基苯胺；2，6-二甲基硝基苯；2，6-二甲基苯胺；3，5-二甲基硝基苯；3，5-二甲基苯胺；丙烯醛；戊二醛等精细化工产品。

Suitable water-immiscible organic solvents include aromatic hydrocarbons, eg toluene, xylene, naphthalene, tetrahydronaphthalene and methyl naphthalene; chlorinated aromatic hydrocarbons, eg chlorobenzene, fluorobenzene, chloronaphthalene and bromonaphthalene; esters, eg butyl acetate, ethyl acetate, methyl benzoate, ethyl benzoate, benzyl benzoate, butyl benzoate, phenylethyl acetate, butyl lactate, benzyl lactate, diethyleneglycol dipropionate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, di(2-ethylhexyl) phthalate; alcohols having six or more carbon atoms, eg hexanol, octanol, benzyl alcohol, phenyl ethanol, phenoxy ethanol, phenoxy propanol and phenoxy butanol; ethers having at least 5 carbon atoms, preferably C 5-14 ethers, eg anisole and phenetol; nitrocellulose, cellulose ether, cellulose acetate; low odour petroleum distillates; turpentine; white spirits; naphtha; isopropylbiphenyl; terpene; vegetable oil; mineral oil; essential oil; and natural oil; and mixtures of any two or more thereof.

适用于水互溶的有机溶剂包括芳香族碳氢化合物，如甲苯，二甲苯，萘，四氢萘和甲基萘；氯代芳香族碳氢化合物，如氯苯，氟，氯萘和萘；酯类，如醋酸丁酯，醋酸乙酯，苯甲酸甲酯，苯甲酸乙酯，苄酯，苯甲酸正丁酯，苯，醋酸丁酯乳酸，乳酸苄，二甘醇二丙酸酯，邻苯二甲酸二甲酯，邻苯二甲酸二乙酯，邻苯二甲酸二丁酯，二（2乙基己基）酯；醇有6个或更多碳原子，如己醇，辛醇，苯甲醇，苯乙醇，苯氧基乙醇，丙醇和苯氧基苯氧丁醇；醚至少有5个碳原子，最好荤5-14醚，如苯甲醚和phenetol；硝化棉，纤维素醚，醋酸纤维素，低气味石油蒸馏；松节油；白酒，石脑油isopropylbiphenyl；萜类，植物油，矿物油，挥发油；和天然油，以及任何两个或两个以上其混合物。

Teflubenzuron was synthesized from 2,4-difluoronitrobenzene and 2,6-dichlobenil as starting reagent through six-step reaction with the yield of 75.3%.3,5-Dichloro-2,4-difluoroaniline was synthesized by chlorination,reduction reaction from 2,4-difluoronitrobenzene,the yield was 84.5%;2,6-difluorobenzamide with the yield of 87.7% was synthesized by fluoridation and hydrolysis from 2,6-dichlobenil.

以2，4-二氟硝基苯和2，6-二氯苯腈为起始原料，经过6步反应合成伏虫隆，总收率为75.3%。以2，4-二氟硝基苯为原料，经过氯化、还原反应合成3，5-二氯-2，4-二氟苯胺，产率为84.5%；以2，6-二氯苯腈为原料，经过氟化和水解，制得2，6-二氟苯甲酰胺，产率为87.7%；将Ⅱ与二碳酸酯酰化，合成2，6-二氟苯甲酰异氰酸酯，产率为91.3%；Ⅲ与Ⅰ加成，得到杀虫剂伏虫隆，产率为95%。

The invention relates to polyimide molding powder with low melt viscosity and a preparation method, which uses 3,4'- diamino diphenyl ether, 3,3',4,4'-diphenyl ketone dicarboxylic anhydride, 3,3',4,4'-biphenyltetracarboxylic dianhydride, 3,3',4,4'- triphenyl diether dicarboxylic anhydride, 3,3',4,4'- diphenyl ether dicarboxylic anhydride and other monomers to polymerize at 100 to 140 DEG C, to get molding powder with a melt viscosity in the range of 1000Pa.s to 5000Pa.s.

本发明属于一种低熔体粘度聚酰亚胺模塑粉及制备方法，是采用3，4′-二氨基二苯醚同3，3′，4，4′-二苯酮四酸二酐、3，3′，4，4′-联苯四酸二酐、3，3′，4，4′-三苯二醚四酸二酐、3，3′，4，4′-二苯醚四酸二酐等单体在100～140℃聚合，获得熔体粘度在1000Pa.s～5000Pa.s范围内的模塑粉。

Water,butylene glycol,cyclomethicone,VP/VA copolymer,glyceryl stearate,glycerin,ppg-15 stearyl ether,titanium dioxide,propylene glycol,cetyl alcohol,citrus aurantium dulcisfruit extract,saccharide isomerate,biosaccharide gum-1,ethoxydiglycol,peg-40 stearate,glycyrrhiza glabraroot extract,morus bombycis root extract,potassium cetyl phosphate,phenoxyethanol,c12-20 acid peg-8 ester,triethanolamine,prunus amygdalus dulcis oil,carbomer,caprylyl glycol,caffeine,disodium edta,methylparaben,chondrus crispus,butylparaben,iris germanica root extract,pentadecalactone,sodium polyacrylate,ethylparaben,sodium hyaluronate,peg-8,propylparaben,citric acid,chlorhexidine digluconate,tocopherol,ascorbyl palmitate,ascorbic acid

水，丁烯二醇，环甲硅脂，VP/VA共聚物，甘油基硬脂酸，甘油，ppg-15 stearyl ether，二氧化钛，丙二醇，十六烷基醇，橙子萃取物，天然异构寡糖， biosaccharde gum-1，乙基氧基乙二醇，聚乙二醇- 40硬脂酸，甘草根提取物，桑白皮根萃取，钾十六烷基磷酸盐，苯氧乙醇，c12-20 acid peg-8 ester，三乙醇胺，甜杏仁油，高分子胶，辛乙二醇，咖啡因，乙二胺四乙酸二钠，对羟基苯甲酸甲酯，卡拉胶，对羟基苯甲酸丁酯，鸢尾花根萃取， pentadecalactone ，聚丙烯酸钠，羟苯乙酯，透明质酸钠，聚乙二醇- 8，羟苯丙酯，柠檬酸，洗必泰葡萄糖酸盐，维生素E，维生素C棕榈酸酯，抗坏血酸

Undecanedioic acid, dodecanedioic acid, brassylic acid, tetradecanedioic acid, pentadecanedioic acid, nylon 1212 resin, nylon 1212 salt, nylon 1212 powder, pa 1212 adhesives and sealants, zirconium dioxide, zirconium dioxide powder, zirconium oxychloride, 1,10-decanediol, 1,12-dodecanediol, dimethyl sebacate, dodecanedioic acid dimethyl ester, dodecane diamine etc.

十一碳二元酸，十二碳二元酸，十三碳二元酸，十四碳二元酸，十五碳二元酸，十二碳二元胺，十二碳二元醇，癸二醇，癸二酸二甲酯，十二碳二酸二甲酯，PA尼龙1212型高档热熔胶；以及二氧化锆，氧氯化锆等。

Three aspects were included here:The derivatives of dihydrol,2,4,5-tetrazine-3,5-dicarboxylic acid were synthesized via three different routes:(1) four new compounds were synthesized via the reaction bet ween dihydrol,2,4,5-tetrazine-3,5-dicarboxylic acid, thionyl chloride and corresponding alcohol ;(2) first ,dimethyl dihydro-1,2,4,5-tetrazine-3,5-dicarboxylate wer e synthesized, then ,another four new compounds were obtained t hrough the alcoholysis under the catalyst ;(3) three acylamines were got through the ammonolysis betw een dimethyl dihydro-1,2,4,5-tetrazine-3,5-dicarboxylate and amines.

本论文分别通过三条不同的路线合成了1，4-二氢-3，6-二甲酸-s-四嗪的衍生物：(1)通过1，4-二氢-3，6-二甲酸-s-四嗪与氯化亚砜和相应的醇反应，制备了四个新化合物；(2)合成1，4-二氢-3，6-二甲酸甲酯-s-四嗪，在催化剂的作用下，与高沸点的醇进行酯交换反应，合成了四个新化合物；(3)合成1，4-二氢-3，6-二甲酸甲酯-s-四嗪后，与胺进行氨解反应，合成三个新的1，4-二氢-3，6-二甲酰胺-s-四嗪化合物。

The chapter two was focused on the samarium diiodide promoted organic reactions and their applications in organic synthesis, firstly, a new synthesis of highly substituted cyclopentadienes from a,β-alkynone promoted by samarium diiodide was investigated and the highly substituted cyclopentadienes were prepared in moderate to good yields under mild conditions. Secondly, the Michael addition and Michael-aldol tandem reaction of diorganyl diselenides or diorganyl disulfides with α,β-alkynones mediated by samarium diiodide were studied and a series of alkenylsulfides and alkenylselenides were prepared in good yields. Then the highly regioselecfive nucleophilic addition of the allylsamarium bromide to α,β-alkynones were explored. We found that the allylsamarium bromide reacts with α,β-alkynones to afford regiospecificly 1. 2-nucleophilic addition products in good yields under mild condition. At last we studied the coupling reaction of aryl halides promoted by NiCl〓/PPh〓/Sm〓.

第二章 研究了二碘化钐、金属钐促进的有机反应：1、二碘化钐促进下α，β-炔基酮的偶联环化反应，提供了一种制备多取代环戊二烯的新方法；2、二碘化钐促进下的二硫醚、二硒醚与α，β-炔基酮的Michael加成反应，为高产率地制备多取代的烯基硫或烯基硒化合物提供了方便可靠的新方法；3、二碘化钐促进下的二硫醚、二硒醚与α，β-炔基酮和醛、酮的Michael—aldol串联反应，提供了一种一锅法高产率地制备多取代的含硫的烯丙基醇或含硒的烯丙基醇类化合物的方便可靠的原子经济性的新方法；4、烯丙基溴化钐与α，β-炔基酮的高度区域选择性的1，2-亲核加成反应；5、NiCl〓/PPh〓/Sm〓促进的卤代芳烃的偶联反应-一种从各种卤代芳烃制备联苯类化合物的有效方法。

The copolycondesation type polyamic acid was synthesized by using pyromellitic dianhydride and 3,3',4,4'-benzophenonetetracarboxylic dianhydride as the dianhydride monomers, 4,4'-diamino diphenylmethane and 4,4'-oxydianiline as the diamine monomers under microwave irradiation in dimethylformamide.

在N，N'-二甲基甲酰胺溶剂中，以均苯四甲酸酐和3，3'，4，4'-二苯酮羧酸二酐为二酐单体，4，4'-二氨基二苯醚和4，4'-二氨基二苯甲烷为二胺单体，采用微波辐射低温溶液共缩聚，合成了聚酰胺酸预聚体，然后亚胺化脱水、环化，生成共缩聚聚酰亚胺。

Dibutyltin maleate,dioctyltin maleate,N-phenyl maleimide, N-(p-chlorophenyl) maleimide,N-(p-nitrophenyl) maleimide with unsaturated groups were synthesized using dibutyltin oxide,dioctyltin oxide,maleic anhydride, aniline,p-chloroaniline,p-nitroaniline as raw materials,respectively.Then dibutyltin male,ate/styrene bipolymer,dibutyltin maleate/styrene/methyl acrylate terpolymer,dibutyltin maleate/styrene/N-phenyl maleimide terpolymer ,dibutyltin maleate/styrene/N-(p-chlorophenyl) maleimide terpolymer ,dibutyltin maleate/styrene/N-(p-nitrophenyl) maleimide terpolymer ,dioctyltin maleate/styrene biopolymer,dioctyltin maleate/styrene/methyl acrylate terpolymer,dioctyltin maleate/styrene/ N-phenyl maleimide terpolymer,dioctyltin maleate/styrene/ N-(p-ehlorophenyl) maleimide terpolymer[P(DOTM/St/NC1PMI)],dioctyltin maleate/styrene/N-(p-nitrophenyl) maleimide terpolymerwere synthesized using DBTO,DOTO,PMI,N-p-ClPMI,N-p-NOPMI,styrene and methyl acrylate as monomers,respectively.

再以DBTO，DOTO，PMI，N-p-ClPMI，N-p-NOPMI，苯乙烯，丙烯酸甲酯等为单体，合成了马来酸二丁基锡/苯乙烯二元共聚物{P}，马来酸二丁基锡/苯乙烯/丙烯酸甲酯三元共聚物{P}，马来酸二丁基锡/苯乙烯/N-苯基马来酰亚胺三元共聚物{P(DBTM/St/NPMI)}，马来酸二丁基锡/苯乙烯/N-对氯苯基马来酰亚胺三元共聚物{P(DBTM/St/NClPMI)}，马来酸二丁基锡/苯乙烯/N-对硝基苯基马来酰亚胺三元共聚物{P(DBTM/St/NNOPMI)}，马来酸二辛基锡/苯乙烯二元共聚物{P}，马来酸二辛基锡/苯乙烯/丙烯酸甲酯三元共聚物{P}，马来酸二辛基锡/苯乙烯/N-苯基马来酰亚胺三元共聚物{P(DOTM/St/NPMI)}，马来酸二辛基锡/苯乙烯/N-对氯苯基马来酰亚胺三元共聚物{P(DOTM/St/NClPMI)}，马来酸二辛基锡/苯乙烯/N-对硝基苯基马来酰亚胺三元共聚物{P(DOTM/St/NNOPMI)}。

Plunder melds and run with this jewel!

掠夺melds和运行与此宝石！

My dream is to be a crazy growing tree and extend at the edge between the city and the forest.

此刻，也许正是在通往天国的路上，我体验着这白色的晕旋。