9,9-二甲基-2-(N-联苯基)氨基芴的合成%Synthesis of N-(4-Biphenyl)-(9,9-Dimethylfluorene-2-y1)amine
河南省科学院化学研究所,郑州,450002 濮阳惠成化工有限公司,濮阳,457001
2010-08-12
9,9-二甲基-2-(N-联苯基) 氨基芴 合成 表征
以芴为原料,苄基三甲基三溴化铵为溴化试剂,室温下在甲醇和二氯甲烷中溴化得到2-溴芴,然后以四氢呋喃为溶剂,在叔丁醇钾作用下与碘甲烷反应合成9,9-二甲基-2-溴芴,最后与4-联苯胺通过Buchwald-Hartwig偶联反应合成目标化合物9,9-二甲基-2-(N-联苯基)氨基芴,总收率为56.0%~62.4%.通过1H NMR 13C NMR、MS、IR和元素分析确证了其结构.%2-Bromofluorene was synthesized with fluorene and benzyltrimethylammonium tribromide in dichloromethane-methanol solution at room temperature,followed by reacting with iodomethane in THF solution in the presence of potassium tert-butanolate,9,9-dimethyl-2-bromofluorene was prepared.At last the titled compound N-(4biphenyl)-(9,9-dimethylfluorene-2-yl) amine was synthesized with 4-aminobiphenyl by the Buchwald-Hartwig reaction.The total yield of the preparation was 56.0%~ 62.4%.All the compounds were characterized by 1 H NMR,13 C NMR,MS,IR spectra and elemental analysis.
