Synthesis and characterization of 2, 7-dibromospiro [fluorene-9, 9'-(2', 7'-dihydroxy-1', 8'-disulfonic-xanthene)]

被引:0
|
作者
Wang L.-Y. [1 ]
Song Y.-J. [1 ]
Cao D.-R. [1 ]
机构
[1] School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, Guangdong
关键词
Fluorene; Spiro; Sulfonation; Synthesis; Yield;
D O I
10.3969/j.issn.1000-565X.2010.09.014
中图分类号
学科分类号
摘要
First, 2, 7-dibromospiro[fluorene-9, 9'-(2', 7'-dihydroxy-xanthene)] (Compound III) was prepared through such three steps as Br2/Fe bromination, CrO3/Ac2O oxidation and resoreinol/ZnCl2 catalytic condensation, with fluorene as the starting material. Then, 2, 7-dibromospiro[fluorene-9, 9'-(2', 7'-dihydroxy-1', 8'-disulfonic-xanthene)] (Compound IV) was synthesized via the sulfonation of Compound III with concentrated sulfuric acid and was characterized by means of IR, 1H NMR and UV-Vis, etc. Finally, the effects of reaction temperature, reactant molar ratio and reaction time on the sulfonation yield were investigated, and the optimal reaction conditions for Compound IV with a yield up to 86.5% were determined, that is, adding 1 g of Compound III together with 3 mL concentrated sulfuric acid for the sulfonation at 70°C for 2 h.
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页码:75 / 79
页数:4
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