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Study On Synthetical Improvement Of 2, 3, 4, 4'-tetrahydroxybenzophenone

Posted on:2007-01-15Degree:MasterType:Thesis
Country:ChinaCandidate:Y W OuFull Text:PDF
GTID:2121360278971679Subject:Pharmacy
Abstract/Summary:PDF Full Text Request
2, 3, 4, 4'—- Tetrahydroxybenzophenone was a very impotant organical and medical intermediate.it was used in many aspects,such as photoresist of integrated circuit, intermediate in medicine, ultra-violet absorption, stabilizer in resin etc.the development and produce will have good perspectives.the way of synthesis refer to reference were zinc chloride catalytic method,resin catalytic method, Boron trifluoride catalytic method etc.the method of Boron trifluoride catalysis had been syudied and improved in this paper.ⅠThe target had been synthesised accoding to reference and proved by spectra analysis such as IR NMR MS.ⅡTo improve the synthetic conditions of the reference,one no poison and cheap solvent X had been found.the product of new method was proved by UV TLC and HPLC analysis.ⅢUse extraction and column chromatography to isolate by-products in new way. one major by-product which is colorless crystal had been isolated and identified namely p-hydroxyl benzoate by spectra analysis such as IR NMR MS.it was proved that the producing way of the major by-product attributed to little alchohol in catalyst.IV After summarizing preliminary experiment, using yield as index orthogonal design was applied to optimize the condition of the newmethod such as temperature,reaction time,catalyst dosage,the materi al ratio.The consequence show that the optimization condition wascatalyst dosage 20ml,temperature 110℃, reaction time 1 hr, P -hydro xybenzcic acid 0.055mol(relative to pyrogallic acid 0.05mol). throug h repeating experimental testing and global evaluation it was provedthat the new method was better than the refrence.
Keywords/Search Tags:2, 3, 4, 4'-tetrahydroxybenzophenone, synthetical improvement, by product isolation, structure identification, orthogonal design
PDF Full Text Request
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