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 Purification of 2-Methyltetrahydrofuran

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PostSubject: Purification of 2-Methyltetrahydrofuran    Wed Aug 03, 2011 8:45 am


The likely impurities of 2-Methyltetrahydrofuran (CAS NO. 96-47-9) are 2-methylfuran, methyldihydrofurans and hydroquinone (stabiliser, which is removed by distn under reduced pressures). It was washed with 10% aqueous NaOH, dried, vacuum distd from CaH2, passed through freshly activated alumina under nitrogen, and refluxed over sodium metal under vacuum. Stored over sodium. Vacuum distd from sodium, and stored with sodium-potassium alloy. (Treatment removes water and prevents the formation of peroxides.) Alternatively, it can be freed from peroxides by treatment with ferrous sulfate and sodium bisulfate, then solid KOH, followed by drying with, and distilling from, sodium, or type 4A molecular sieves under argon. It may be difficult to remove benzene if it is present as an impurity (can be readily detected by its ultraviolet absorption in the 249-268nm region). It has also been purifed by percolating through A12O3 and fractionated collecting fraction b 79.5-80 °C. After degassing, the material was distd onto degassed molecular sieves, then distd onto anthracene and a sodium mirror. The solvent was distd from the green soln onto potassium mirror or sodium-potassium alloy, from which it was distilled again. It should be stored in the presence of 0.1% of hydroquinone as stabiliser.
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