水溶性噻吩衍生物(3-噻吩)乙氧基丁基磺酸盐的合成
HRP-catalyzed synthesis of water-soluble polythiophene PTEBS
以3-溴噻吩为原料,经格氏反应制得格式试剂,而后与环氧乙烷反应,合成了3-噻吩乙醇。生成的3-噻吩乙醇和氢化钠反应形成钠盐后再和1,4-丁磺酸内酯反应,合成(3-噻吩)乙氧基丁基磺酸盐(TEBS)。并对每一步产物进行了检测和分析。实验发现,当3-溴噻吩与镁粉的摩尔比为1:1.5时,格氏收率达到90%以上,而格氏试剂与环氧乙烷反应时的温度越低,3-噻吩乙醇的收率越高,同时溶剂四氢呋喃的量较大对反应有利,3-溴噻吩在四氢呋喃中的浓度低于5mol/L时,3-噻吩乙醇的收率达到70%以上。在制备TEBS过程中,溶剂甲苯的量是影响TEBS产率的关键因素。
he Grignard reagent is made from the raw material 3-bromothiophene through Grignard reaction. Then the Grignard reagent reacts with ethylene oxide to generate 3-thiophene ethanol. The obtained 3-thiophene ethanol reacts with sodium hydride to form sodium salt which then reacts with 1, 4-Butane sultone, generating (3-thiophene) ethoxy butyl sulfonate (TEBS). Detect and analyze every step of the product.It was found that the Grignard yield more than 90% when the molar ratio of 3 - bromothiophene and magnesium powder is 1:1.5, the lower the temperature, the higher the 3 - thiophene ethanol yield when Grignard reagent reaction with ethylene oxide that,large amount of THF is good on the reaction,the yield of 3 - thiophene ethanol is more than 70% when 3 - bromothiophene in THF concentrations below 5mol / L.In the process of preparation TEBS,The amount of the solvent toluene is a key factor to affect the yield of TEBS.
王兴涌、舒芳亮
有机化学工业精细化学工业
格氏反应3-噻吩乙醇水溶性噻吩
Grignard reaction3-thiophene ethanolwater-soluble thiophene
王兴涌,舒芳亮.水溶性噻吩衍生物(3-噻吩)乙氧基丁基磺酸盐的合成[EB/OL].(2012-02-16)[2025-08-19].http://www.paper.edu.cn/releasepaper/content/201202-600.点此复制
评论