Font Size: a A A

Microwave Radiation And Phase Transfer Catalytic Synthesis Of Three ¦Â-nitro Styrene

Posted on:2005-09-17Degree:MasterType:Thesis
Country:ChinaCandidate:G Y LiFull Text:PDF
GTID:2191360125955429Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
β-Nitro substituted styrenes are important primary materials or intermediates,and posses significant biological activities such as insecticidal ,fungicidal ..bactericidal and antitumor agents.They have been synthesized by Henry reaction with two new kinds of technology (microwave irradiation,MWI and phase transfer catalysis,PTC) in this paper.PTC is an important method in organic synthesis reactions.It can shorten reaction time and increase yields.Through a series of experiments,the choice of optional PTC reagent,PTC reagent amount,reaction temperature,reaction time and the molar ratio of reactants were investigated. The results showed that under the optinal reaction conditions in which the reaction for 4-hydroxy- β-methyl- B -nitrostyrene underwent for 1.5h at 80℃,with PEG-1000 as PTC reagent, the yield of product was 85.8%.and in which the reaction for 4-methoxy-β-methyl- β-nitrostyrene underwent for 2h at 90℃,with A-1 as PTC reagent,the yield of product was 75.2%.and in which the reaction for p-chloro- β-nitrostyrene underwent for 2h at 78℃, with A-l as PTC reagent, the yield of product was 74.3%.MWI is a new technology in organic synthesis. The shorter reaction time and expanded reaction range that is offered by microwave assisted organic synthesis are suited to the increasing demands in industry. In this paper,the effects of different factors such as the power of microwave irradiation and reaction time were studied.The results indicated the microwave irradiation could shorten reaction time greatly.In the same time,MWI and PTC were applied simultaneously in the reaction system.Through a series of experiments, the effects of different factors such as the power of microwave irradiation ,reaction time,different PTC activity,PTC reagent amount and the molar of reactant were researched.The experiment results showed that the reaction for 4-hydroxy-β-methyl-β-nitrostyrene underwent for 5min at 195W with PEG-800 as PTC reagent, the yield was 70.5%,that the reaction for 4-methoxy- β-methyl- β-nitrostyrene underwent for 8min at 130W withPEG-1000 as PTC reagent, the yield was 48.9%.These two methods have been proved to be successful in this paper.
Keywords/Search Tags:microwave irradiation, phase transfer catalysis, 4-hydroxy-β-methyl-β-nitrostyrene, 4-methoxy-β-methyl-β-nitrostyrene, p-chloro- β-nitrostyrene
PDF Full Text Request
Related items