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Silica-supported Palladium Coupling Reaction Catalyzed By Organic Tin And Chloride Of Ph <sub> 2 </ Sub> The Sncl <sub> 2 </ Sub> And The Reaction Of Xanthate,

Posted on:2004-02-09Degree:MasterType:Thesis
Country:ChinaCandidate:Y MaFull Text:PDF
GTID:2191360092993695Subject:Organic Chemistry
Abstract/Summary:PDF Full Text Request
This dissertation consists of two parts: Part one:A silica-supported poly y -disphenylphosphinopropyl siloxane-palladium complex has been prepared by better method and has been found to catalyze the cross-coupling reaction of organotins with acid chlorides.The experimental results show that the silica-supported phosphine palladium complex is the effective catalyst to this kind of cross-coupling reaction.The reaction conditions, which comprised the selection of the solvent, the dosage of the solvent and the catalyst, the reaction time and the injection of the inertia gas, has also been discussed and the best reaction condition has been found, which the molecular ratio of the palladium and acid chloride is 1.52x10-2:1 organotin and acid chloride reflexed for 20 hours in chloroform has made the result. Also this reaction does not need the presence of the inertia gas. At last, the products were validated by melting point, IR, UV, 1HNMR. The experiment has testified that the polymeric catalyst was stable and could be easily separated from a reaction mixture and reused. The polymeric could be reused for 5 times before it lost the catalytic activity.Part two:A new synthesis method of 2,2,4,4,6,6-Hexaphenyl-l,3,5-trithia -2A6-tristannacylclohexan(Ph2SnS)3 has been found. The reaction between Diphenylzindichloride Ph2SnCl2 and Potassium (o-ethyl dithiocarbonate) resulted in two products under different condition . At lower temperature we can gain (EtOCS2)2SnPh2. If the temperature has been raised to about 80 ℃ , (Ph2SnS)3 was the main product. Through the parallel experiment which has been done with (EtOCS2)2SnPh2Cl. We guess that (EtOCS2)2SnPh2 is the intermediates of the (Ph2SnS)3.
Keywords/Search Tags:Silica-supported
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