苯并[1,2-d:5,4-d']二(噁唑)-2,6-二硫醇的合成及表征  

Synthesis and Characterization of Benzo[1,2-d: 5,4-d']bis( oxazole)-2,6-dithiol

作　　者：颜瑞[1,2] 罗一鸣[1] 江国庆[2] 唐瑞仁[1] 李星[2] 姜国民[2] 

机构地区：[1]中南大学化学化工学院,湖南长沙410083 [2]南通大学化学化工学院,江苏南通226019

出　　处：《化学试剂》2016年第8期787-790,共4页Chemical Reagents

基　　金：国家自然科学基金资助项目(21173122);江苏省高校自然科学研究计划项目(14KJB150018)

摘　　要：苯并噁唑类化合物是一类重要的杂环化合物,不仅在生物、医药等方面有着广泛应用,而且在光学材料、高性能复合材料等诸多领域也显现出独特的性能。以间苯二酚为原料,经过酯化反应和Fries重排、肟化反应、Beckmann重排和水解反应合成4,6-二氨基间苯二酚盐酸盐(DAR·HCl)。然后以4,6-二氨基间苯二酚盐酸盐和二硫化碳为原料合成标题化合物,并且优化了过程的工艺条件,过程的总收率为37.3%。利用红外光谱、核磁共振谱、质谱和元素分析等分析手段对中间产物及目标化合物进行了表征。Benzobisoxazole compounds are the basic structural unit of poly（ p-phenylene-benzobisoxazole）,which have superior tensile strength,modulus and thermal stability. Benzobisoxazole compounds are mainly used in optoelectronic materials,medicine synthesis and coordination chemistry. Using resorcinol as raw material,4,6-diaminoresorcinol dihydrochloride（ DAR·2HCl） was synthesized by esterification,fries rearrangement,oximation,Beckmann rearrangement and hydrolysis. Benzo[1,2-d： 5,4-d＇]bis（ oxazole）-2,6-dithiol was prepared by cyclization between 4,6-diaminoresorcinol dihydrochloride and carbon disulfide,the conditions of the process were optimized and the overall yield was 37. 3%. The intermediate products and the target product were characterized and confirmed by FT-IR,1HNMR,elemental analysis and HPLC-MS.

关 键 词：间苯二酚 4 6-二氨基间苯二酚盐酸盐 苯并[1 2-d:5 4-d']二(噁唑)-2 6-二硫醇 合成 表征 

分 类 号：O626.2[理学—有机化学]