Feng Qing
2009
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Journal
Journal of Zhejiang University of Technology
Abstract
1,2,3,9-tetrahydro-9-methyl-4H-carbzol-4-one(CAR) has been synthesized by nitration,hydrogenation and cyclization using N-methylaniline and 1,3-cyclohexanedione as raw materials and HMCM-41 as a catalyst.The influences of the temperature of cyclization,catalyst concentration,molar ratio of reagent and solvent were investigated.Optimum synthesis conditions were obtained as follow: reaction temperature was 60 ℃;catalyst concentration(PH/catalyst) was 0.3;molar ratio of reagent(CH/PH) was 1.2,and solvent was methanol.The yield of CAR was 65.3%.The final product(HPLC≥99.0%) was obtained by re-crystallization using the proper acetone-water solution.