胺化

A photoresist composition including a polymer is disclosed, wherein the polymer includes at least one monomer having the formula: wherein, R1 is selected from H, linear, branched or circular alkyl with 1-20 carton atoms, linear, branched or circular alkyl with 1-20 C atom, which is perfluorinated or semi-perfluorinated; and CN; R2 is alicyclic group with 5 or more carbon atoms; X is selected from methylene, aether, ester, amide and the connecting part of the carbonate; R3 is linear or branched alkylene with one or more carbon atoms or perfluorinated or semi-perfluorinated linear or branched alkylene; R4 is selected from H, CH3, CF3, CHF2, CH2F and perfluorinated or semi-perfluorinated aliphatic group; R5 is selected from the CF3, CHF2, CH2F and perfluorinated or semi-perfluorinated substituted and unsubstituted aliphatic group; n is 1 or higher integer; OR12 is OH or at least an acid unstable group selected from the tert-alkyl carbonate, tert-alkyl ester, tert-alkyl aether, acetal and ketal.

本发明公开了一种包含一种聚合物的光刻胶组合物，该聚合物包括至少一种具有下列结构的单体：其中，R 1 选自氢、具有1～20个碳原子的线形、支化或环状烷基、半氟化或全氟化的具有1～20个碳原子的线形、支化或环状烷基、以及CN；R 2 为具有5个或更多个碳原子的脂环基团；X为选自亚甲基、醚、酯、酰胺和碳酸酯的连接部分；R 3 为具有1个或多个碳原子的线形或支化亚烷基或者半氟化或全氟化的线形或支化亚烷基；R 4 选自氢、甲基(CH 3 )、三氟甲基(CF 3 )、二氟甲基(CHF 2 )、氟代甲基(CH 2 F)、以及半氟化或全氟化的脂族基团；R 5 选自三氟甲基(CF 3 )、二氟甲基(CHF 2 )、氟代甲基(CH 2 F)、以及半氟化或全氟化的取代或未取代的脂族基团；n为1或更大的整数；OR 12 为OH或者选自叔烷基碳酸酯、叔烷基酯、叔烷基醚、缩醛和缩酮的至少一种酸不稳定基团。

Part 2. Annulation reaction of 3, 4-dichlorocoumarin (1) and 3, 4-dichloromaleimide (8) by a new general annulation strategy developed in this group with 2-phenylbenzofuran (15), 3-phenylbenzofuran (16), 2, 5-diphenyloxazole (17), 2, 5-diphenylthiazole (18), 2-methyl-4-phenylthiazole (19) and 2, 3-dimethoxy-1, 3-butadiene (40) were investigated.

二。在本课题组前一阶段提出的从二氯代环烯酮与1，1-二芳基乙烯的光化反应以及光化反应中得到的环丁烷产物的连续电环化反应对3，4-二氯马来酰亚胺以及3，4-二氯香豆素进行增环反应的工作基础上，研究了3，4-二氯香豆素（1）和3，4-二氯马来酰亚胺（8）与5个α-苯基取代的环烯烃2-苯基苯并呋喃（15），3-苯基苯并呋喃（16），2，5-二苯基噁唑（17），2，5-二苯基噻唑（18），2-甲基-4-苯基噻唑（19），以及一个丁二烯——2，3-二甲氧基丁二烯（40）进行的芳香族增环反应。

Goal compound synthesis namely: Take the vanillic acid as outset raw material, obtains 4- hydroxyl - 3- anisole methyl formate with the methyl alcohol reflux conditions, then after the etherification, the nitration, the return to original state, the ring closure response obtains 6- methoxy - 7- animal pen oxygen radical kui zuo lin - 4- alkone, then passes through the chlorination, the substitution aniline, to escape responses again and so on animal pen oxygen radical, etherification to obtain the goal compound; The goal compound and the diethylamine had the amine substitution reaction to obtain TM1, namely 4- benzene amino - 6- methoxy - 7- [2- hydroxyl - 3-(N, N- two ethyl aminos) third oxygen radical] kui zuo lin; Through zuo has the etherification with the Austria niter to respond obtains TM2, namely 4- benzene amino - 6- methoxy - 7- [2- hydroxyl - 3-(2- methyl - 5- nitryl imidazole) third oxygen radical] kui zuo lin.

目标化合物的合成即：以香草酸为起始原料，与甲醇回流条件下得到4-羟基-3-甲氧基苯甲酸甲酯，然后经过醚化、硝化、还原、环合反应得到6-甲氧基-7-苄氧基喹唑啉-4-酮，然后再经氯化、取代苯胺、脱苄氧基、醚化等反应得到目标化合物；目标化合物与二乙胺发生胺取代反应得到了TM1，即4-苯氨基-6-甲氧基-7-[2-羟基-3-丙氧基]喹唑啉；通过与奥硝唑发生醚化反应得到TM2，即4-苯氨基-6-甲氧基-7-[2-羟基-3-(2-甲基-5-硝基咪唑)丙氧基]喹唑啉。

Synthesis of target compounds namely: to vanillic acid as the starting material with methanol under reflux conditions for 4 - hydroxy -3 - p-methyl, then ether, and nitration, reduction, cyclization reaction 6 - methoxy -7 - benzyloxy-quinazoline -4 - one, and then by the chloride in place of aniline, benzyloxy-off, such as etherification reaction of the target compounds; target compounds with the second and third occurrence of substitution reactions of amines by the TM1, that is, 4 - amino-benzene -6 - methoxy -7 - [2 - hydroxy -3 -(N, N-diethyl amino) oxy c] quinazoline; with ether occurred Ornidazole reaction of TM2, namely, 4 - amino-benzene -6 - methoxy -7 - [2 - hydroxy -3 -(2 - methyl -5 - nitroimidazole) C oxy] quinazoline.

本论文以嘌呤类似物喹唑啉为母核，分别在其4位和7位引入结构多样的取代苯氨基和柔性侧链，设计了一系列4-取代苯胺基-6-甲氧基-7-(2-羟基取代丙氧基)喹唑啉类化合物。目标化合物的合成即：以香草酸为起始原料，与甲醇回流条件下得到4-羟基-3-甲氧基苯甲酸甲酯，然后经过醚化、硝化、还原、环合反应得到6-甲氧基-7-苄氧基喹唑啉-4-酮，然后再经氯化、取代苯胺、脱苄氧基、醚化等反应得到目标化合物；目标化合物与二乙胺发生胺取代反应得到了TM1，即4-苯氨基-6-甲氧基-7-[2-羟基-3-丙氧基]喹唑啉；通过与奥硝唑发生醚化反应得到TM2，即4-苯氨基-6-甲氧基-7-[2-羟基-3-(2-甲基-5-硝基咪唑)丙氧基]喹唑啉。

DDS was used as test drug for determination of acetylator phenotype employing HPLC.The results showed that both the occupational and non-occupational exposed group were predominantly slow acetylators(52.2％and 45.5％),higher than that in the exposed controls(13.0％)(0 05).The risks for bladder cancer with the slow ace...

结果表明。无论有无2－萘胺职业接触史，膀胱癌病人中慢型乙酰化者所占比例（52.2％和45.5％）均高于对照组（13.0％），且差异有显著性（P＜0.05），比值比0R分别为5.56（95％可信限＝1.02～30.3）和7.25（95％可信限＝1.70～30.3），提示慢型乙酰化者若暴露于2－萘胺更易患膀胱肿瘤，乙酰化慢表型是膀胱癌的一个遗传易感因素。

Study on an efficient process for the preparation of trifloxystrobin starting from 2-methylacetophenone bypartial oxidation,esterification,reaction with methoxyamine,bromization and condensation with 3'- acetophenone oxime.

以邻甲基苯乙酮为原料，经过高锰酸钾的碱性氧化，甲醇酯化，再与甲氧基胺盐酸盐肟化后，用N-溴丁二酰亚胺溴化，最后和间三氟甲基苯乙酮肟缩合得到目标产物肟菌酯。

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。

Was synthesized from succimide by bromination with bromine,methylation with dimethyl sulfate and the reaction of indolyl magnesium bromide with 2,3-dibromoN-methylmaleimide.

以琥珀酰亚胺为起始原料，经过溴化、甲基化后再与吲哚溴化镁加成反应合成了2-溴-3-(1H-吲哚-3)-N-甲基马来酰亚胺，总收率44.8%，其结构经1H NMR和IR确证。

To economize cost of S03H-functionalized ionic liquids,extend their range of application in chemistry reaction,fifteen of ionic liquids have been synthesized by using methylimidazole,tri-alkylamine,pyridine with industrial materials 1,4-butane-sultone and 1,3-propane sultone as source in this paper.The ionic liquids were synthesized by tri-alkylamine have not been reported and yields are higher than 98%.

为了降低SO_3H-功能化离子液体的成本，使其应用范围更加广泛，本论文利用N-甲基咪唑、三烷基胺、吡啶和廉价工业级原料1，3-丙烷磺内酯、1，4-丁烷磺内酯为原料来源，合成十五种SO_3H-功能化离子液体，三甲胺为原料合成的SO_3H-功能化离子液体还未见文献报道，收率大于98%。

Two series of polyurethane acrylate grafted acrylic resins (Acr-g-TPU-PETA and Acr-gPPU-PETA) self-emulsifying systems are obtained by grafting -NCO group modified polyurethane acrylates with acrylic copolymer prepared from n-butyl acrylate, styrene,βhydroxyethyl methacrylate and acrylic acid The self-emulsifying systems showed Newtonian fluidity with viscosity closed to that of water, the solid contents were around 30% The T〓 of 15～4℃ for dried film before photocuring favored film formation at room temperature DSC and DMA results showed that PU-PETA is compatible with acrylic resin in the grafted resin The TG and dTG curves for Acr-g-PU-PETA samples were substantially different from the corresponding blends, and the brodened dTG peaks for photocured grafted resin suggest that there might be multiple interactions among chain segments The photocued film of the grafted resins self-emulsifying system exhibited good overall properties with polyurethane acrylate grafts ranging from 30% to 50%, and Acr-g-TPU-PETA series showed better properties than Acr-gPPU-PETA series The adhesion of the photocured film was 1～2 grade, impact strength was 50kg-cm and flexibility was 1mm The Shore hardness and the adhesion of the film decreased markedly if PETA was replaced by HEMA as photoactive group due to the lower C=C double bond content in the grafted resin The polyhydroxy amine-linked thioxanthones photoinitiators can be evenly dispersed in self-emulsifying system without color spot appearing in the dried film The films photocured with IV〓～IV〓 generally exhibited higher Shore hardness, gloss and solventresistance than that cured with Irgacure 2959 and did not induce the rusting of the iron substrate Pigmenting with titanium oxide had no effect on the photocuring The polyhydroxy amine-linked thioxanthone IV〓 and IV〓 can be new candidates for the formulation of titanium oxide pigmented photocurable water-borne coatings for their pale-yellow appearance and slight interference with the color of the coatings WB 4759 with high water-solubility coalesced and separated from the dried resin film, and even induced the rusting of iron substrate.

以丙烯酸丁酯，甲基丙烯酸-β-羟乙酯，丙烯酸及苯乙烯合成厂丙烯酸共聚树脂，并与含-NCO端基的聚氨酯丙烯酸酯接枝反应，经水性化后，得到两个系列（Acr-g-TPU-PETA和Acr-g-PPU-PETA）各5个不同配比的丙烯酸树脂接枝聚氨酯丙烯酸酯自乳化体系，粘度与水相近，为牛顿流体，固含量30％左右。光固化前干燥涂膜的玻璃化转变温度在-15℃～4℃之间，有利于室温下成膜。DSC及DMA谱表明两种树脂基本相容。Acr-g-PU-PETA的热失重行为明显不同于共混材料，接枝样dTG峰明显宽化，表明接枝样中链段之间的相互作刚有多重性，丙烯酸树脂与聚氨酯之间有一定的相容性。接枝树脂自乳化体系光固化涂层的综合性能以聚氨酯丙烯酸酯成分为50％～30％者相对较好，且以Acr-g-TPU-PETA系列更理想。光固化膜的附着力为1～2级，冲击强度为50kg·cm，柔软性多为1mm。以HEMA代替PETA作为接枝树脂的活性基团，碳—碳双键密度太低，光固化膜交联点太少，硬度和附着力均较差。多羟基胺连硫杂蒽酮光引发剂能均匀分散于树脂自乳化体系和接枝树脂干膜中，不出现色斑，光固化膜肖氏硬度一般高于以Irgacure 2959为光引发剂的光固化膜，光泽度及耐丁酮溶剂性能均有所提高，不会诱导铁基生锈，钛白着色对光固化结果几乎没有影响。本论文所合成的多羟基胺连硫杂蒽酮光引发剂IV〓与IV〓为浅黄色，对光固化涂层的颜色干扰较小，为配制钛白着色光固化水性涂料提供了新的光引发剂。水溶性太强的WB 4759在干膜中易聚结析出，且对所附着的铁基有诱导锈蚀作用。

The split between the two groups can hardly be papered over.

这两个团体间的分歧难以掩饰。

This approach not only encourages a greater number of responses, but minimizes the likelihood of stale groupthink.

这种做法不仅鼓励了更多的反应，而且减少跟风的可能性。