1，6－己二硫醇的合成研究

以１，６－二溴己烷为原料，合成了一种重要的鸡肉味香料１，６－己二硫醇，产率８５．０％。同时报道了一种简便的以１，６－己二醇为原料制备１，６－二溴己烷的方法，产率８９．５％。     

1，6－二溴己烷的合成研究

１，６－二溴己烷是一种重要的有机合成中间体，对其合成方法进行了研究，产率达到８０．５％。     

1－溴－4－溴甲基苯的简易合成及应用

以对溴甲苯为原料，Ｎ－溴代丁二酰亚胺为溴化剂，利用光引发的自由基反应合成了１－溴－４－溴甲基苯，产率可达８０％，并利用它制得了一个新的有机金属前体。     

18—冠—6的合成

用钾离子为模板，采用稀释法，以三甘醇和３，６－二氧－１，８－二氯辛烷为原料，经Ｗｉｌｌｉａｍｓｏｎ反应合成了１８－冠－６，并用硝基甲烷进行提纯。考察了反应时间，反应物配比，氢氧化钾加入方式对产率的影响。实验结果表明；反应时间为２０ｈ，三甘醇和三甘醇的二氯化物的物质的量比为１．１：１，氢氧化钾粉状加入时，１８－冠－６的产率可达５１．５８％。产物的结构红外光谱及熔点确认。     

2，6－二溴－1，5－二羟基萘的合成

以萘为原料，经磺化、羟基化、溴化反应合成了２，６ 二溴 １，５ 二羟基萘，并对工艺条件进行了研究。其中磺化步１，５ 二磺化产物收率达７２６％，溴化步２，６ 二溴 １，５ 二羟基萘收率达９３６％。     

苄基三乙基氯化铵相转移催化合成N,N-二己基邻乙基苯胺的研究

采用苄基三乙基氯化铵为相转移催化剂，以邻乙基苯胺为原料、１－溴己烷为烷基化试剂，常压下合成了Ｎ，Ｎ－二己基邻乙基苯胺，并研究了反应物摩尔比、催化剂用量、反应时间对目的产物产率的影响，确定了实验设计范围内的最佳工艺条件。目标化合物的结构经ＩＲ和１ＨＮＭＲ谱图解析确认。     

2，6－二溴－1，5－二羟基萘的合成

以萘为原料，经磺化、羟基化、溴化反应合成了２，６二溴１，５二羟基萘，并对工艺条件进行了研究。其中磺化步１，５二磺化产物收率达７２６％，溴化步２，６二溴１，５二羟基萘收率达９３６％。     

2-氨基-4-溴-5-氯苯甲酸的合成

以硝基苯为原料，经溴化、还原、缩合、环合、氯化和氧化等６步反应合成了２－氨基－４－溴－５－氯苯甲酸，总收率为１１．７％。     

7,16—二硫苯并18—冠—6的新合成法

目前,对以苯并１８－冠－６为中间体的双冠醚的研究很多［１］,而对含硫的苯并１８－冠－６及其双冠醚的研究则几乎没有,其主要原因是含硫的苯并１８－冠－６合成难,产率很低,文献［２］报道的７,１６－二硫苯并１８－冠－６的产率还不到１％。我们参照文献［３］合成氮杂冠醚的方法来合成硫杂冠醚,得到了高纯度、较高产率的７,１６－二硫苯并１８－冠－６。此法产率较高,产物的分离和纯化也较简便,其合成路线如下：（　）２ＯＯＴｓＯＯＴｓＨＳＯＳＨｔ－ＢｕＯＨ／二氧六环,碱ＯＳＯＯＳＯ１　实验部分１．１　试剂和仪器苯二…     

1—溴—4—溴甲基苯的简易合成及应用

以 对溴甲苯为原料，Ｎ－溴代丁二酰亚胺为溴化剂，利用光引发的自由基反应合成了１－溴－４－溴甲基苯，产率可达８０％，并利用它制得了一个新的有机合金属前体。     

4′-(6-溴己氧基)联苯-4-甲酸甲酯的合成

4′ 羟基联苯 4 甲酸与甲醇反应,合成了4′ 羟基联苯 4 甲酸甲酯。后者与1,6 二溴己烷反应合成了目标化合物4′ (6 溴己氧基)联苯 4 甲酸甲酯,反应工艺条件为:以无水乙醇为溶剂,n(4′ 羟基联苯 4 甲酸甲酯)∶n(碳酸钾)∶n(1,6 二溴己烷)=1∶1 5∶3,80℃反应8h,收率达60 8%。两步总收率57 6%。目标化合物经IR,1HNMR和元素分析确证了分子结构。     

A practical Ti-salen catalyst based on dimeric salen ligand for asymmetric addition of trimethylsilyl cyanide to aldehydes

A dimeric salen ligand derived from L-tartaric acid was synthesized through linking two salen units with 1,6-dibromohexane. The corresponding Ti complex was proved to be an efficient catalyst for asymmetric addition of trimethylsilyl cyanide to aldehydes, providing the corresponding optically active trimethylsilyl ether of cyanohydrins with moderate to good enantiomeric excesses and excellent yields under relatively low catalyst loading condition.     

4-(6-氨基己氧基)-4′-氰基联苯的合成

以4-羟基-4′-氰基联苯(Ⅰ)为原料,在碳酸钾(水和乙醇作溶剂)溶液中与1,6-二溴己烷反应得到4-(6-溴己氧基)-4′-氰基联苯(Ⅱ),然后经过Gabriel反应、肼解反应制得4-(6-氨基己氧基)-4′-氰基联苯(Ⅳ)。与国外相似结构的合成工作相比,简化了反应步骤,且总收率由文献[2]的27.8%提高到55.2%。用IR、1HNMR和元素分析确证了目标产物的化学结构;经DSC测试,其液晶相转变温度为:Tm(熔点)83℃,Ti(清亮点)104℃。为了应用和贮存将其转变为相应的盐酸盐。     

Aromatic-aliphatic polysulfides. Products of the polycondensation of 4,4′-bis(mercaptomethyl)biphenyl with some dihalogen hydrocarbons

Polysulfides were synthesized by high-temperature solution polycondensation of 4,4′-bis(mercaptomethyl)biphenyl with selected aliphatic and aromatic-aliphatic dihalogen hydrocarbons. To determine the optimum polycondensation conditions, the influence of the following factors on reduced viscosity and yield were studied: type of organic solvent, type of hydrogen halide (HX) acceptor, concentration of reagents, reaction temperature and reaction time. A through examination was carried out only for the polycondensation of dithiol with bis(4-chloromethylphenyl)methane and 1,6-dibromohexane chosen as model system. The structures of polysulfides were confirmed by elemental analysis, X-ray analysis and infrared spectroscopy. The temperature of initial decomposition, the percentage of its mass loss, and the temperature of the fastest decomposition process were determined from the curves of differential and thermogravimetric analysis. Some physicochemical, mechanical and electrical properties were determined.     

相转移催化法合成19,19,26,26-四十四烷基四羧酸四乙酯

研究了以丙二酸二乙酯、l,6-二溴己烷为原料,以十六烷基三甲基溴化铵(CTMBA)和聚乙二醇(PEG-1000)为协同相转移催化剂,在一定条件下首先合成了非离子Gemini表面活性剂中间体1,1,8,8-辛基四羧酸四乙酯,进而通过加原料溴代十八烷于1,1,8,8-辛基四羧酸四乙酯中,在相同催化剂条件下合成了标题化合物....     

新型表面印迹材料MIP-P4VP/SiO2对谷氨酸对映体的手性拆分

引言氨基酸作为构成蛋白质分子的基本单位,是构成人体的最基本物质之一,是生命代谢的物质基础,在人的营养和健康中有着不可替代的作用。在生命科学研究领域,氨基酸对映体的拆分具有十分     

Mg-mediated Copolycondensation of α,α-Dibromotoluene with Bifunctional Electrophiles

Copolycondensation of α,α-dibromotoluene (1) with α,α‘-dibromo-p-xylylene (2) was found to proceed in the presence of excess Mg via nucleophilic substitution of in situ generated Grignard reagents to Br-bearing benzylic carbons. The use of dichlorodimethylsilane (3) and 1,6-dibromohexane (4) as a comonomer in the ternary copolycondensation with 1 and 2 was effective to give higher molecular weight polymers by improving their solubility. In the series of the copolycondensation, the copolymer with the highest M _n of 8480 was obtained in a 41% yield by the reaction of a feed ratio of [1]:[2]:[4] = 1:1:1 in THF at room temperature.     

二（N，N－二乙基甘氨酸）-1，6-己二醇酯的合成

SnC12作催化剂,1,6-已二醇和氯乙酸在环己烷中网流3h获得1,6-已二醇双氯乙酸酯,然后再与二乙胺在室温下反应3h,合成了新化合物二（N,N-二乙基甘氨酸）-1,6-已二醇酯,总产率达71．8％,并对影响1,6-已二醇双氯乙酸酯产率的因素进行了探讨。     

Novel ionenes with allyl pendant groups

Summary Novel ionenes with allyl pendant groups have been synthesized by condensation of N,N'- bisallylpiperazine with organic dihalides such as 1,4-dichlorobutane, 1,6-dibromohexane and 1,4-dichloromethylbenzene. The polymers are readily soluble in water and have low molecular weights. The structure of the ionenes has been identified by spectroscopic techniques. The concentrated aqueous solutions of the resulting ionenes can be crosslinked by t-butylhydroperoxide as a radical initiator to give transparent hydrogels. The ionenes also act as an crosslinking agent in copolymerization with high concentrations of acrylic acid in the presence of K₂S₂O₈ as a radical initiator in water at 65°C. Received: 29 July 1999/Revised version: 28 October 1999/Accepted: 28 October 1999