甲基溴

Two bispyrazolylimine nickel complexes [bis-N-(phenyl-1,3,5-dimethylpyrazolylmethylene) phenylimine nickel dibromide] (Cat.1) and [bis-4-methoxy-N-(phenyl-1,3,5-dimethylpyrazolylmethylene) phenylimine nickel dibromide] (Cat.2) were synthesized.

合成了两种双吡唑亚胺镍配合物：双－N-（苯基－1-3，5-二甲基吡唑基亚甲基）苯基亚胺二溴化镍Cat.1）和双－4-甲氧基－N-（苯基－1-3，5-二甲基吡唑基亚甲基）苯基亚胺二溴化镍

In our research on study chemical reaction of active methylene compounds and brom-acetophenone. Because of brom-acetophenone is compound that contain carbonyl and halogen ,which will take place electrophilic substitution and nucleophilic addition. When active methylene compounds are ethyl acetoacetate and β-diketone, controlling reaction condition, we have found that mono-substitution's production and di-substitution's. production is isolated; active methylene compounds are acetoacetanilide and acetoacetanilide derivate, pyrrolidin-2-one derivants were obtained by substitution and close-ring reaction .but there is no report about it.

本文是让活泼亚甲基类化合物与溴代苯乙酮发生化学反应，由于溴代苯乙酮是含有羰基的卤代烃结构，它可以发生亲电取代和亲核加成反应，当活泼亚甲基类化合物为乙酰乙酸乙酯和β-二酮时，控制反应条件可以发生单取代和双取代两种产物；当活泼亚甲基类化合物为乙酰乙酰芳胺类化合物来反应时，溴代苯乙酮中的羰基与氨基会发生分子内的关环反应生成吡咯烷-2-酮衍生物，这在以前的研究中是没有发现的。

A selective and mild PS-DIB/ionic-liquid immobilized 2, 2, 6, 6-tetramethyl-piperidin-4-ol-N-oxyl catalytic oxidation procedure of alcohols to the corresponding aldehydes and ketones in ionic liquid BF4 at room temperature was developed. The oxidant PS-DIB was prepared via the iodation and acetylation of polystyrene resin. For the preparation of the ionic-liquid immobilized TeMPO catalyst, 4-(2, 2, 6, 6-Tetramethyl-1-oxyl-4-piperidoxyl)butyl bromide was first synthesized from TeMPO and 1, 4-dibromobutane.

将聚苯乙烯树脂先碘化再乙酰基化，制得了负载型二乙酰氧碘苯作为氧化剂。2， 2， 6， 6-四甲基－N-氧自由基哌啶醇与1， 4-二溴丁烷反应生成4-溴丁氧基－2， 2， 6， 6-四甲基－哌啶－1-氧化物，再与N-甲基咪唑发生季铵化反应，生成的溴化季铵盐与四氟硼酸钠进行离子交换制得氟硼酸型2， 2， 6， 6-四甲基－N-氧自由基哌啶负载离子液体。

A selective and mild PS-DIB/ionic-liquid immobilized TEMPO catalytic oxidation procedure of alcohols to the corresponding aldehydes and ketones in ionic liquid BF4 at room temperature was developed. The oxidant PS-DIB was prepared via Iodation and acetylation of polystyrene resin. For the preparation of the ionic-liquid immobilized TEMPO catalyst, 4-(2,2,6,6-Tetramethyl-1-oxyl-4-piperidoxyl)butyl bromide was first synthesized from 2,2,6,6-tetramethyl-piperidin-4-ol-N-oxyl and 1,4-dibromobutane.

将聚苯乙烯树脂先碘化再乙酰基化，制得了负载型二乙酰氧碘苯(diacetoxyiodo polystyrene，PS-DIB)作为氧化剂。2，2，6，6-四甲基-N-氧自由基哌啶醇(2，2，6，6-tetramethyl-piperidin-4-ol-N-oxyl，TEMPO)与1，4-二溴丁烷反应生成4-溴丁氧基-2，2，6，6-四甲基-哌啶-1-氧化物，再与N-甲基咪唑发生季铵化反应，生成的溴化季铵盐与四氟硼酸钠进行离子交换制得氟硼酸型2，2，6，6-四甲基-N-氧自由基哌啶负载离子液体TEMPO-IL。

Ethoxycarbonyl-4,5-dimethyl-pyrrole (7) was prepared from ethylacetoacetate, ethyl formate and methyl ethyl ketone via oximination, Claisen condensation, and reductive condensation. The bromization of compound 7 gave 2-ethoxycarbonyl-3-bromo-4,5-dimethyl-pyrrole(8), which could be transferred to 2-ethoxy-carbonyl-3-brome-4-methyl-5-formyl-pyrrole (9) by the formolation.

由乙酰乙酸乙酯、甲酸乙酯及丁酮等原料经过肟化、Claisen缩合、还原缩合成环得到2-乙氧羰基－4，5-二甲基－吡咯(7)，溴化生成2-乙氧羰基－3-溴4，5-二甲基－吡咯(8)，最后经过甲酰化反应得到目标产物2-乙氧羰基－3-溴－4-甲基－5-甲酰基－吡咯(9)。

Tetrachloroterephthalic acid was prepared by chlorinating terephthalic acid, oleumsolvent and iodine catalyst. Tetrachloroterephthalic acid was acylated by sulphurous oxychloride in the presence of DMF to form tetrachloroterephthaloyl chloride. The acyl chloride product was fluorinated by potassium fluoride and esterified by methanol to synthesize dimethyl tetrafluoroterephthalate. The ester was reduced with potassium borohydride and lithium chloride to give tetrafluoroterephthalyl alcohol. The above product was bromated in the hydrobromic acid to obtain 4-bromomethyl-2,3,5,6-tetrafluoro-benzene methanol. 4-Methyl-2,3,5,-6-tetrafluorobenzene ethanol was obtained by reducing the bromide with magnesium. In the exist of DCC and DMAP, tefluthrin was got by the condensation reaction between 4-methyl-2,3,5,6-tetrafluoro-benzene methanol and-(1RS,3RS)- 3-(2- chloro-3,3,3-trifluoro-1-propenyl)-2,2-dimethyl cycolpropanecar-boxylate acid.

对苯二甲酸与氯气在碘存在下以发烟硫酸为溶剂进行氯化制备四氯对苯二甲酸；再以DMF为催化剂与二氯亚砜反应生成四氯对苯二甲酰氯；以氟化钾为氟化剂，环丁砜为溶剂置换氟化，再与甲醇酯化得到四氟对苯二甲酸甲酯；以KBH4-LiCl为还原剂二甲醚为溶剂反应制得四氟对苯二甲基苄醇；以氯苯为溶剂在溴化氢溶液中溴化得到溴化产物；在乙醇溶液中经镁粉还原得到4-甲基-2，3，5，6-四氟苄醇；甲基苄醇与功夫酸在催化剂二环己基碳二亚胺和4-二甲氨基吡啶作用下缩合得到七氟菊酯，总收率达43.6%。

Their structures were characterized by IR, 1H NMR, of which 4-chloro- 2-methyl-7-(2-bromoethoxy) isoflavone, 2, 4\'-dimethyl-7-(2-bromo-ethoxy)isoflavone and 2-methyl-7-(2-bromoethoxy) isoflavone are rarely reported so far.4\'-chloro-2-methyl-7-(3-bromopropoxy)isoflavone, 2, 4\'-dimethyl-7-(3-bromo- propoxy) isoflavone, 2-methyl-7-(3-bromopropoxy) isoflavone, 4\'-methoxy-2-methyl-7-(3-bromopropoxy) isoflavone and 4\'-hydroxy-2-methyl-7-(3-bromopropoxy) isoflavone were gained by reacting 7-hydroxy-2-methyl isoflavone derivatives with 1, 3-dibromo- propane, respectively.

第三章(来源：73ABC论文网www.abclunwen.com)在丙酮溶液中以K_2CO_3为碱，使溴乙氧基异黄酮和溴丙氧基异黄酮与咪唑偶合，以较高的产率合成出10种目标化合物：2-甲基-4′-氯-7-2-(1-咪唑基乙氧基异黄酮、2，4′-二甲基-7-2-(1-咪唑基乙氧基异黄酮、2-甲基-7-2-(1-咪唑基乙氧基异黄酮、2-甲基-4′-甲氧基-7-2-(1-咪唑基乙氧基异黄酮、2-甲基-4′-羟基-7-2-(1-咪唑基乙氧基异黄酮、2-甲基-4′-氯-7-3-(1-咪唑基丙氧基异黄酮、2，4′-二甲基-7-3-(1-咪唑基丙氧基异黄酮、2-甲基-7-3-(1-咪唑基丙氧基异黄酮、2-甲基-4′-甲氧基-7-3-(1-咪唑基丙氧基异黄酮、2-甲基-4′-羟基-7-3-(1-咪唑基丙氧基异黄酮，经IR、~1H NMR、~(13)C NMR、元素分析等对其结构进行了表征，10种目标产物均未见文(来源：ABC论文cccccc网www.abclunwen.com)献报道。

The bromo-polyethylenegylcol-monomethacrylate was synthesized by two steps. Firstly, methylacrylic acid was esterified with polyethylene glycol (PEG, M=200, 400) to give polyethyleneglycol-monomethacrylate Secondly, treatment of PEG-MA with phosphorus tribromide gave the aim product.

以聚乙二醉（M分别为200，400）和甲基丙烯酸进行单酯化反应，所得单酯再与三溴化磷进行溴化反应合成了一种新的两端具有功能团的不饱和溴化物，即溴代甲基丙烯酸单聚乙二醇酯。

Bromo-5-formyl -3-methylpyrrole is an important intermediate of tolyporohin. On the base of introducing the present research and development of tolypo- rohin and pyrroles ramification at home and abroad, an emphasis was made on synthesis of 2-Bromo-5-formyl -3-methylpyrrole and the technical conditions of all steps, which was described as follows.

由于2-溴-5-甲基-3-甲基咯是合成托尼吩的重要中间体，本文在阐述了当前托尼吩及咯衍生物的国内外研究和开发的基础上，重点研究了2-溴-5-甲基-3-甲基咯的合成，并对各步反应进行了工艺研究，具体合成步骤如下：本文通过对乙乙酸乙酯的亚硝化、还原、成环，反应生成咯单环衍生物2，4-二乙氧羰基-3，5-二甲基咯。

N-methylmaleimide was prepared by using dimethyl sulfate as methylation reagent.The paper investigated the addition of N-methyl-3,4-dibromomaleimide and indolylmagnesium bromide,and then 2-bromo-3-(1H-indolyl-3-yl)-N-methylmaleimide and 3,4-bis(1H-indolyl-3-yl-)-N-methyl-maleimide were obtained.

对吲哚在溴乙烷和镁作用下生成吲哚溴化镁，而后与3，4－二溴－N－甲基马来酰亚胺的加成反应进行了研究，合成了2－溴－3－(1H－吲哚－3)－N－甲基马来酰亚胺，并对反应条件进行了改进，研究了反应温度和原料配比对反应的影响。

And discuss some key point of integrated management system design, include hazard identification and risk assessment and risk control in the occupational health and safety management, the measure of satisfaction target of customer, the flawlessness of law system, the integration of the integrated management system and enterprise standardization system, unify lead institution and work orgnization, integreted internal audit and integrated management review.

同时，论述了一体化管理体系构建中的几个主要问题，包括职业健康安全管理中的危险源辨识、风险评价和风险控制、顾客满意度的科学监测、法律、法规体系的完善、一体化管理体系与企业标准化体系的有机结合、统一的领导机构和工作机构、一体化的内部审核和管理评审。

Deepwater Taranaki is investigated for its petroleum potential, using all available seismic data tied to shallow-water wells.

运用与浅水井相关的现有全部震波探测数据考察了深海区塔拉纳基盆地的油藏前景。