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luofengping铜虫 (小有名气)
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[求助]
请教一溶剂问题
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大家帮我看看下面的文献,能不能将里面的硝基甲烷用四氢夫喃,因为我按一下文献做,产物得不到要的物质,我首先怀疑是不是溶剂的问题,或者是AlCl3 的问题?To a solution of 3 (0.3 g) in dry nitromethane (10 mL) was added AlCl3 (0.45 g) under nitrogen. After stirring the mixture for 0.5 h, DDQ (0.38 g) in dry nitromethane (5 mL) was added dropwise and the solution was stirred at r.t. for 1 h. A solution of 2 N HCl was added with stirring. The resulting mixture was extracted with CH2Cl2 (325 mL). The combined extracts were dried (Na2SO4), the CH2Cl2 was distilled off, and the residue was flash chromatographed using petroleum ether and ethyl acetate (6:1, v/v) as eluent. A white powder 4 (0.23 g) was obtained in 77% yield; |
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2楼2007-11-06 09:12:27
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