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求助DMSO的精制!!!!
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| 求助DMSO的精制!!!!文献上只简单说经CaH2加热处理后,在氮气保护下减压蒸馏,但没说具体怎么做,求助呀!!! |
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samuel01
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Dimethyl sulfoxide (DMSO) [67-68-5] M 78.1, m 18.0-18.5°, b 75.6-75.8°/12mm, 190°/760mm, d 1.100, n 1.479. Colourless, odourless, very hygroscopic liquid, synthesised from dimethyl sulfide. The main impurity is water, with a trace of dimethyl sulfone. The Karl-Fischer test is applicable. It is dried with Linde types 4A or 13X molecular sieves, by prolonged contact and passage through acolumn of the material, then distd under reduced pressure. Other drying agents include CaH2, CaO, BaO and CaSO4. It can also be fractionally crystd by partial freezing. More extensive purification is achieved by standing overnight with freshly heated and cooled chromatographic grade alumina. It is then refluxed for 4h over CaO, dried over CaH2, and then fractionally distd at low pressure. For efficiency of desiccants in drying dimethyl sulfoxide see Burfield and Smithers J Org Chem 43 3966 1978\ Sato et al. J Chem Soc, Dalton Trans 1949 1986]. Rapid purification: Stand over freshly activated alumina, BaO or CaSO4 overnight. Filter and distil over CaH2 under reduced pressure (~ 12 mm Hg). Store over 4A molecular sieves. 以上见elsevior 的试剂纯化手册第5版 [ Last edited by samuel01 on 2007-1-23 at 20:38 ] |
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