Zhao De-feng
2006
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0
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Journal
Journal of Dalian University of Technology
Abstract
2-Hydroxy-4-methoxy-3′-nitrodibenzophenone(3) is prepared from the Friedel-Crafts acylation reaction of 1,3-dimethoxybenzene(1) with meta-nitrobenzoyl chloride(2).The yield of dibenzophenone is 71.8%,while CH_2Cl_2 is used as solvent,the reaction temperature is 40 ℃,the reaction time is 3 h,and the molar ratio of AlCl_3 and 1,3-dimethoxybenzene to meta-nitrobenzoyl chloride is 3∶1.1∶1.The conversion of 3 to 2-hydroxy-4-methoxy-3′-aminodibenzophenone(4) is carried out by catalytic hydrogenation over 5% Pd/C in 90.2% yield.Monoalkyl(91.4%)and dialkyl(88.9%) derivatives of compound 4 are afforded with methylsulphate as alkylation agent.The structure of the final products and several key intermediates are identified by IR,()~1H NMR and mass spectum.