重氮化法合成9，9-二苯基芴

采用盐酸重氮化法合成9,9-二苯基芴。以9，9-双（4一氨基苯基）芴为原料，在0~20~C下重氮化，反应分别采用亚硝酸正加法，亚硝酸反加法反应，用次磷酸还原脱除重氮盐合成9,9-二苯基芴。对次磷酸的用量、盐酸的配比以及反应温度进行了探究。浓盐酸重氮化合成9,9-二苯基芴，HPLC显示副反应较多，硅胶柱层析（淋洗剂PE：EA=15：1）可得到白色9,9-二苯基芴，纯度：98％（HPLC），熔点224～226~C，收率可达52．3％。

Synthesis of 9, 9-Diphenyl-9H-Fluorene by the Diazotization Reaction of 4, 4＇-（9H-Fluorene-9, 9-Diyl） Dianiline

The hydrochloric acid diazotization method was adopted for the synthesis of 9, 9-diphenyl fluorene. The 4, 4＇-（9H-fluorene-9, 9- diyl） dianiline as raw material was diazotized with nitrite at 0-20℃ by positive and negative method, and then reduced by hypophosphorous acid to remove diazonium salt so as to synthesize 9,9-biphenyl fluorene. The hypophosphorous acid dosage, the ratio of hydrochloric acid, and reaction temperature were studied. The concentrated hydrochloric acid was added into diazonium compounds to synthesize 9,9-biphenyl fluorene. The HPLC displayed there were many side reactions. After the separation by silica gel column chromatography （eluting agent PE ： EA=15 ： 1 ）, the white 9,9- biphenyl fluorene was obtained with a melting point of 224-226 ~C and a purity of 98% , the yield was up to 52.3%.