Title: Synthesis of 2-Methyl-2-Hydroxy-1-Phenyl-1-Pentanone
Abstract: First,2-methyl isocaproyl chloride was prepared by 2-methylvaleric acid and thionyl chloride.Second,2-methyl-1-phenyl-1-pentanone was synthesized with benzene and isocaproyl chloride in the presence of anhydrous aluminum chloride as a catalyst.Then,2-methyl-2-hydroxy-1-phenyl-1-pentanone was prepared by chlorination and hydrolysis with 2-methyl-1-phenyl-1-pentanone in the presence of NaOH and CCl4 as chlorinating agent and tetrabutyl ammonium bromide as the phase transfer catalyst.The result shows:when n(2-methylvaleric acid)/n(thionyl chloride) is 1.0∶1.5,dropwise temperture and time of thionyl chloride is 40 ℃ and 1.5 h respectively,reaction time is 2.5 h,anhydrous aluminum chloride is 18.5 g,benzene is 45 mL,dropwise time of isocaproyl chloride is 0.5 h,the yield of 2-methyl-1-phenyl-1-pentanone is 92.7%;when n(2-methyl-1-phenyl-1-pentanone)/n(CCl4) is 1.0∶1.8,tetrabutyl ammonium bromide is 6 g,mass fraction of sodium hydroxide is 20% and reaction time is 5 h,the yield of 2methyl-2-hydroxy-1-phenyl-1-pentanone can be up to 91%.The structure of the product was characterized by elemental analysis,IR and MS.
Publication Year: 2007
Publication Date: 2007-01-01
Language: en
Type: article
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