ILIAS CHEMISTRY - M.E.S. Indian School,Doha
Would you like to react to this message? Create an account in a few clicks or log in to continue.

ILIAS CHEMISTRY - M.E.S. Indian School,Doha

This is a forum for the students of MES, to get note and ask doubts to the chemistry department of the school.
 
HomeLatest imagesSearchRegisterLog in

 

 Purification of 3-Picoline

Go down 
AuthorMessage
happybaicaitou
New Student
New Student



Posts : 4
Join date : 2011-08-26

Purification of 3-Picoline  Empty
PostSubject: Purification of 3-Picoline    Purification of 3-Picoline  Icon_minitimeTue Aug 30, 2011 3:24 am

3-Picoline (CAS NO. 108-99-6) often contains 4-methylpyridine and 2,6-lutidine, neither of which can be removed satisfactorily by drying and fractionation, or by using the ZnCl2 complex. Biddiscombe and Handley after steam distn as for 2-methylpyridine, treated the residue with urea to remove 2,6-lutidine, then azeotropically distd with acetic acid (the azeotrope had b 114.5 °C/712mm), and recovered the base by adding excess of aqueous 30% NaOH, drying with solid NaOH and carefully fractionally distilling. The distillate was then fractionally crystd by slow partial freezing. An alternative treatment is to reflux the crude base (500mL) for 20-24h with a mixture of acetic anhydride (125g) and phthalic anhydride (125g) followed by distn until phthalic anhydride begins to pass over. The distillate was treated with NaOH (250g in 1.5L of water) and then steam distd. Addition of solid NaOH (250g) to this distillate (ca 2L) led to the separation of 3-methylpyridine which was removed, dried (K2CO3, then BaO) and fractionally distd. (Subsequent fractional freezing would probably be advantageous.)
Back to top Go down
 
Purification of 3-Picoline
Back to top 
Page 1 of 1
 Similar topics
-
» Purification of 2-Methyltetrahydrofuran
» Purification of 1-Propanol
» Purification of 2-Methylpyridine
» Purification of Nitromethane
»  Purification of Isobutanol

Permissions in this forum:You cannot reply to topics in this forum
ILIAS CHEMISTRY - M.E.S. Indian School,Doha :: Chat with your Teacher :: Doubts on Related Topics-
Jump to: