Welcome to LookChem.com Sign In | Join Free

Details

Home > Chemical Encyclopedia > Chemical Technology > Laboratory Chemical Technology >
 Purification of 2,6-Lutidine
  • Purification of 2,6-Lutidine
  • Likely contaminants of 2,6-Lutidine (CAS NO. ) include 3- and 4-picoline (similar boiling points). However, they are removed by using BF3, with which they react preferentially, by adding 4mL of BF3 to 100mL of dry fractionally distd 2,6-lutidine and redistilling. Distn of commercial material from AlCl3 (14g per 100mL) can also be used to remove picolines (and water). Alternatively, lutidine (100mL) can be refluxed with ethyl benzenesulfonate (20g) or ethyl p-toluenesulfonate (20g) for 1h, then the upper layer is cooled, separated and distd. The distillate is refluxed with BaO or CaH2, then fractionally distd, through a glass helices-packed column.

    2,6-Lutidine can be dried with KOH or sodium, or by refluxing with (and distilling from) BaO, prior to distn. For purification via its picrate, 2,6-lutidine, dissolved in abs EtOH, is treated with an excess of warm ethanolic picric acid. The ppte is filtered off, recrystd from acetone (to give m 163-164.5 °C), and partitioned between ammonia and CHCl3/diethyl ether. The organic soln, after washing with dilute aqueous KOH, is dried with Na2SO4 and fractionally distd. 

    Alternatively, 2,6-lutidine can be purified via its urea complex, as described under 2,3-lutidine. Other purification procedures include azeotropic distn with phenol, fractional crystn by partial freezing, and vapour-phase chromatography using a 180-cm column of polyethylene glycol-400 (Shell, 5%) on Embacel (May and Baker) at 100 °C, with argon as carrier gas.


    Prev:No record
    Next:No record
  • Back】【Close 】【Print】【Add to favorite
Periodic Table
    Hot Products