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The present invention relates to plastic fire retardant preparing technology, and is especially process of preparing pentabromo benzyl bromide.

本发明属于塑料加工用阻燃剂技术领域,具体涉及一种五溴苄基溴的制备方法。

A new chiral quaternary ammonium salt 1a was synthesized by the reaction of cinchonine and(2,4,6-)trimethyl benzyl chloride.Etherification between 1a and benzyl bromide,allyl chloride,or methyl give corresponding etherified quaternary ammonium salts 1b,1c,and 1d.

由辛可宁和2,4,6-三甲基苄氯,合成了一种新的手性季铵盐(1a),并进一步用苄基溴、碘甲烷和烯丙基氯对分子中的羟基进行醚化,得到相转移催化剂1b、1c和1d。

Benzyl bromide was synthesized from potassium bromide ,a by-product from synthesis of 2-hydroxy-4-n-octyloxybenzophenone(UV-531),and benzoic alcohol in the presence of concentrated sulfuric acid.

溴化钾作为工业生产2-羟基-4-正辛氧基二苯甲酮的副产品,在浓硫酸存在的条件下,与苯甲醇进行反应合成苄基溴

In part one, the reactions of some active fluorine-containing compounds such as 2, 2-dihydropolyfluoroalkanoic acids and ethyl 2-hydropolyfluoroalkenoates were studied and various fluorine-containing heterocyclic compounds were synthesized. Using 2, 2-dihydropolyfluoroalkanoic acids as the starting material, 4-fluoroalkyl quinolin-2-ols, 2- [ -1-hydropolyfluoro-1-alkenyl] -4H-3, 1-benzoxazin-4-ones, 1-aryl -4, 9-dihydro-3-fluoro-alkyl-1H-pyrazo [3, 4-b] quinolin-4-ones, 5-fluoroalkyl-12H-quin olino [2, 1-b] quinazolin-12-ones, 4-fluoroalkyl-1, 3-dihydro-1, 5-benzodiazepin-2-ones and 4-fluoroalkyl-2H-pyrido [1, 2-a] pyrimidin-2-ones were synthesized through its condensation reaction with anilines, anthranilic acid, N'-aryl-o-aminobenzamides, o-nitro aniline, o-amino pyridine and their derivatives and the subsequent transformations. 5-Fluoroalkyl isoxazolidines, 3-fluoro-3-fluoroalkylisoxazolidino [4, 3-c] quinolin-4-ones, 3-fluoroalkylisoxazolino [4, 3-c] quinolin-4-ones and 2-aryl-3per fluoroacylindoles were synthesized by inter-and intramolecular 1, 3-dipolar cycloaddition of fluorine-containing olefins and nitrones.

第二部分,我们研究了α,α-二氟苄基卤类化合物的亚磺化脱卤反应、产物的转化及全氟烷基亚磺酸盐与芳环化合物的全氟烷基化反应,发现全氟苄基碘或溴及α,α一二氟苄基溴在保险粉等亚磺化脱卤试剂引发下可生成相应的亚磺酸盐;全氟苄基亚磺酸盐与氯气或溴反应可生成全氟苄基磺酰氯或磺酰溴;在烯烃存在下,全氟苄基碘则与烯烃发生加成反应,生成相应的1:1加成产物;在三价醋酸锰的作用下,部分芳香化合物如茴香醚,二甲氧基苯,吡啶,喹啉等可以和过量的全氟烷基亚磺酸盐发生双全氟烷基化反应,反应表现出一定的区域选择性,产率良好。

Bromination occur s selectively on the PMS methyl group, providing a reactive benzylic bromine functionality which is the key to Exxpro specialty elastomers′ vulcanization and modification versatility.

溴化反应选择性地发生在PMS的甲基基团上,提供活性苄基溴官能团,这也是Exxpro特种弹性体硫化和各种改性的关键。

Fourteen new pyrethroids containing isoxazole were designed and synthesized from 4-isopropyl-3-substituted phenyl-5-hydroxyl isoxazoles as major material, whose structures were also characterized by IR, 1H NMR and elemental analysis.

以4-异丙基-3-取代苯基-5-羟基异噁唑和3-苯氧基苄基溴为原料,三乙胺为缚酸剂,设计并合成了14个未见报道的4-异丙基-3-取代苯基-5-异噁唑基-(3'-苯氧基)苄基醚。通过红外光谱、核磁共振、元素分析等手段,确证了它们的化学结构。

The experimental results showed that there were higher yield and bromine content when the bromine/peroxides method was used.

采用溴/过氧化物法和NBS法对五溴甲苯进行苄位溴化,合成了五溴苄基溴,比较了两种方法的优缺点。

An unusual substitution of 5-fluorouracils by the reaction of lithium salts of 1,3-dialkyl-5-fluorouracil with benzyl bromide is described.

1,3-二烷基-5-氟尿嘧啶的锂盐与苄基溴进行苄基化反应时产生了异常的反应结果。

The prepared pentabromo benzyl bromide may be applied in preparing high efficiency fire retardant.

制备的五溴苄基溴可用于制备五溴苄基丙烯酸酯或烷基醚类聚合物用高效阻燃剂。

The process includes the following steps: dissolving bromine in halogenated hydrocarbon, dropping the bromine solution into reactant system comprising pentabromo toluene, halogenated hydrocarbon, free radical initiator and hydrogen peroxide at 50-65 deg.c, and heating to 60-78 deg.c for reflux reaction until the reactant system becomes transparent; filtering the resultant to obtain solid product, washing with carbon tetrachloride and water separately and vacuum drying to obtain pentabromo benzyl bromide.

具体步骤为:将五溴甲苯、卤代烃、自由基引发剂和过氧化氢组成的反应体系加入到三颈瓶中,将0.07~0.1mol的溴溶于50ml卤代烃配成溶液,在50-65℃温度下滴加到反应体系中,滴加时间为50-70分钟,然后升温至60-78℃温度下回流反应,至反应体系逐渐变透明,且不再产生气泡时,将所得产物过滤,得到固体产物,分别用CCl 4 和水洗涤,真空干燥,即得到五溴苄基溴;其中,五溴甲苯与溴的摩尔比为1∶0.7-1∶1.0,溴与过氧化氢的摩尔比为1∶1.0-1∶1.4,自由基引发剂加入量为五溴甲苯重量的1-10%,卤代烃的加入量为反应体系体积的40%-100%,所用溶剂可以直接进行下一批反应,不需要更换溶剂或蒸馏提纯。

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