Preparation of Dess-Martin periodinane - The role of the morphology of 1-hydroxy-1,2-benziodoxol-3(1H)-one 1-oxide precursor
Preparation of Dess-Martin periodinane - The role of the morphology of 1-hydroxy-1,2-benziodoxol-3(1H)-one 1-oxide precursor
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DOI：
10.1039/a605253c
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发表时间：
1997
期刊：
影响因子：
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通讯作者：
P. Stevenson;Alan B. Treacy;M. Nieuwenhuyzen
中科院分区：
文献类型：
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作者：
P. Stevenson;Alan B. Treacy;M. Nieuwenhuyzen
通过用溴酸钾氧化邻碘苯甲酸制备的1-羟基-1，2-苯碘酰-3（1H）-酮1-氧化物形成微晶粉末、粗晶材料或两种形式的混合物。这种物理形式上的差异是难以将1-羟基-1，2-苯碘酰-3（1H）-酮1-氧化物可再现地转化为相应的I-三乙酰氧基衍生物的根源。本文介绍了一种将1-羟基-1，2-苯碘酰-3（1H）-酮1-氧化物晶体转化为活性更高的粉末形式的简单方法。微晶粉末和粗晶材料通过X射线衍射表征。
1-Hydroxy-1,2-benziodoxol-3(1H)-one 1-oxide prepared by oxidation of o-iodobenzoic acid with potassium bromate forms either a microcrystalline powder, a macrocrystalline material, or a mixture of both forms. This difference in physical form is the source of the difficulty in reproducibly converting 1-hydroxy-1,2-benziodoxol-3(1H)-one 1-oxide to the corresponding I-triacetoxy derivative. A simple method is given for conversion of crystalline 1-hydroxy-1,2-benziodoxol-3(1H)-one 1-oxide to the more reactive powder form. The microcrystalline powder and macrocrystalline material are characterised by X-ray diffraction.