One-pot Synthesis of 4-Phenyl-6-Methyl-5-Ethoxycarbonyl-3,4-Dihydropyrimidin-2(H)-one with H_4SiW_6Mo_6O_(40)/SiO_2
Yang Shui-ji
Abstract
Yang Shui-ji
Abstract
A new catalyst,H4SiW6Mo6O40/SiO2was prepared by a sol-gel technique.Using H4SiW6Mo6O40/SiO2as catalyst,4-phenyl-6-methyl-5-ethoxycarbonyl-3,4-dihydropyrimidin-2-(H)-one was synthesized via one-pot method reaction from ethyl acetoacetate,with benzaldehyde,urea and anhydrous ethanol as solvent.The influence factors of reaction conditions on the yield of the product were discussed and the best reaction conditions were shown as follows:under the condition of fixed benzaldehyde consumption is 0.04mol and anhydrous ethanol is 15mL,n(benzaldehyde):n(ethylacetoacetate):n(urea)is 1∶1.2∶1.5,reaction temperature is 90℃,mass fraction of catalyst to reactants is 2.5%and reaction time is 90min.The yield of the product can reach 72.3%.The 3,4-dihydropyrimidin-2(H)-one was characterized by melting point measurements,IR,HNMR and MS spectroscopy.
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A new catalyst,H4SiW6Mo6O40/SiO2was prepared by a sol-gel technique.Using H4SiW6Mo6O40/SiO2as catalyst,4-phenyl-6-methyl-5-ethoxycarbonyl-3,4-dihydropyrimidin-2-(H)-one was synthesized via one-pot method reaction from ethyl acetoacetate,with benzaldehyde,urea and anhydrous ethanol as solvent.The influence factors of reaction conditions on the yield of the product were discussed and the best reaction conditions were shown as follows:under the condition of fixed benzaldehyde consumption is 0.04mol and anhydrous ethanol is 15mL,n(benzaldehyde):n(ethylacetoacetate):n(urea)is 1∶1.2∶1.5,reaction temperature is 90℃,mass fraction of catalyst to reactants is 2.5%and reaction time is 90min.The yield of the product can reach 72.3%.The 3,4-dihydropyrimidin-2(H)-one was characterized by melting point measurements,IR,HNMR and MS spectroscopy.
Key concepts: Benzaldehyde, Yield (engineering), Anhydrous, Catalysis, Chemistry, Urea, Ethanol, Ethyl acetoacetate