J. Jing
2013
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Journal
Fine chemicals
Abstract
5-Bromo-7,7-dimethyl-7H-benzo[C]fluorine was prepared from 1-bromonaphthalene in 63.1% yield.The synthetic process of intermediates 2-(1-naphthalenyl)benzaldehyde,7-methyl-7H-benzo[C]fluorene and,7-dimethyl-7H-benzo[C]fluorene were optimized.The optimum conditions were as follows.In the synthesis of 2-(1-naphthalenyl)benzaldehyde,when the amount of catalyst Pd(dppf)Cl2 was 3.0%,reaction temperature was 40 ℃ and reaction time was 2 h,the yield was 96.8%.In the synthesis of 7-methyl-7H-benzo[C]fluorene,when the amount of catalyst Amberlyst 15 ion-exchange resin was 0.6%,reaction temperature was 110 ℃ and reaction time was 4 h,the yield was 95.4%.In the synthesis of 7,7-dimethyl-7H-benzo[C]fluorene,when n(methyl 4-methylbenzenesulfinate)∶n(7-methyl-7H-benzo[C]fluorene)=2.5∶1 and reaction temperature was 40 ℃,the yield was 91.0%.The product was characterized by means of 1HNMR and ESI-MS.