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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。

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)。

A process for preparingp-fluo-2-(2-methyl-3-propionyl)-4-oxy-N,3-diphenyl-phenylbutylamide includes such steps as Friedle-Craft acylating of newly prepared phenylacetyl chloride and fluorobenzene under catalysis of AlCl3 to obtain 4-fluoro-phenylbenzyl ketone, brominating at carbonyl alpha position under catalysis of less AlCl3 to obtain alpha-bromo-4-fluo-phenylbenzyl ketone, and condensing with isobutyryl acetanilide under action of sodium ethoxide.

本发明涉及一种制备对氟-2-(2-甲基-3-氧丙基)-4-氧-N,3-二苯基-苯丁酰胺(1)的方法,其包括以下步骤:新制的苯乙酰氯与氟苯在AlCl3催化下进行Friedle-Craft酰化反应,得到对4-氟-苯基苄基酮(4);化合物(4)在少量AlCl3催化下进行羰基α位溴化,得到α-溴-4-氟-苯基苄基酮(5);然后(3)异丁酰乙酰苯胺在乙醇钠作用下与化合物(5)进行缩合。

In order to decrease toxicities of retinods and enhance pharmacal effects and gain the relative derivatives with better curing effect and selectivity, structures of retinoic acids were modified by inducing glycosyl groups in this paper.

方法一是在氢氧化钾存在下,以4-二甲氨基吡啶做相转移催化剂,将溴代-O-乙酰基葡萄糖(5a)、溴代-O-乙酰基木糖(5b)、溴代-O-乙酰基乳糖(5c)和溴代-O-乙酰基麦芽糖(5d)分别与异维A酸反应制得1-O-异维A酰-乙酰基单糖(6a,6b)和1-O-异维A酰-乙酰基二糖(6c,6d),收率为53~65%。

The famciclovir was synthesized from purine by a series of steps by Acylation, Decarboxylation, Reduction ,and so on; Derivatives of these intermediates is described from the 6-chloro- 9H- purin-2-amine as raw materials in different conditions when the iodine and bromide were synthesized with the addition of two intermediate 6-bromo-9H-purin-2-amine and 6-iodo-9H-purin-2-amine; There is elaborated from the main part of a acetophenone, urineaminohydrochloride, phenylhydrazine, ethyl acetoacetate as raw material through a series of reactions to synthetic 3-phenyl-4-formylphenyl pyrazole and 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-aldehyde two pyrazole aldehyde, and then with 2-amino-6-chlorine-9-(2-methicillin-oxo-co-methyl-4-yl) purine reaction of the two new pyrazole purine Schiff bases.

本论文主是采用以鸟嘌呤为原料,经过一系列的酰基化,脱羧,还原等反应作用下最终得到了产物2-氨基-9-(4-乙酰氧基-3-乙酰氧基甲基丁基)嘌呤;其中的中间体衍生物主要是阐述从以2-氨基-6-氯鸟嘌呤为原料通过在不同的条件下进行溴代与碘代分别合成了另外两种中间体2-氨基-6-溴鸟嘌呤及2-氨基-6-碘鸟嘌呤;还有一部分主要是阐述从以苯乙酮,盐酸氨基脲,苯肼,乙酰乙酸乙酯为原料通过一系列的反应先合成3-苯基-4-醛基吡唑及5-氯-3-甲基-1-苯基-1H-吡唑-4-甲醛这两个吡唑醛,然后再与2-氨基-6-氯-9-(2-甲氧羰基丁酸甲酯-4-基)嘌呤反应得到了两个新型的吡唑嘌呤席夫碱

It is found that when the molar ratio of sulphoxide,pyridine and acetyl bromide is 1∶0.6∶0.4,the catalytic effect on the ring-enlargment is the best,and the yield and purity of the final product can reach 76% and 97% respectively at a pH of 1.8 in toluene under refluxing for about 3.5h.

通过正交实验可得出以下结论:当N,N′-双脲-亚砜为2.5∶1,乙酰溴-亚砜为0.4∶1,吡啶-乙酰溴为1.5∶1,回流时间为3.5h,酸化pH值为1.8时,扩环反应结果最好,总收率可达76%,纯度97%以上。

For example, pulverized wood samples can be treated with acetyl bromide in acetic acid, and the absorbance of the resulting solution at 280 nm can be compared with the absorbance obtained from known lignin standards.

例如,将木屑样品在乙酸环境下与乙酰溴进行反应,再将280纳摩尔所得溶液的吸收率与已知的木质素标准吸收率进行比较。

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. Diethyl 3,5-dimethylpyrrole-2,4-dicarboxylate was made by nitrification, reduction and cycle of ethyl acetoacetate.

由于2-溴-5-甲酰基-3-甲基吡咯是合成托尼卟吩的重要中间体,本文在阐述了当前托尼卟吩及吡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-甲酰基-3-甲基吡咯的合成,并对各步反应进行了工艺研究,具体合成步骤如下:本文通过对乙酰乙酸乙酯的亚硝化、还原、成环,反应生成吡咯单环衍生物2,4-二乙氧羰基-3,5-二甲基吡咯。

The effect of chloroacetyl chloride and bromoacetyl bromide on yields of intermediates and nitrazepam was compared.

比较了氯乙酰氯和溴乙酰溴对中间体及硝基安定收率的影响。

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According to the clear water experiment, aeration performance of the new equipment is good with high total oxygen transfer coefficient and oxygen utilization ratio.

曝气设备的动力效率在叶轮转速为120rpm~150rpm时取得最大值,此时氧利用率和充氧能力也具有较高值。

The environmental stability of that world - including its crushing pressures and icy darkness - means that some of its most famous inhabitants have survived for eons as evolutionary throwbacks, their bodies undergoing little change.

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