- Purification of N,N-Dimethylaniline
-
Primary and secondary amines (including aniline and monomethylaniline) can be removed by refluxing for some hours with excess acetic anhydride, and then fractionally distilling. Crocker and Jones used four volumes of acetic anhydride, then distd off the greater part of it, and took up the residue in ice-cold dil HCl. Non-basic materials were removed by ether extraction, then the (CAS NO. ) was liberated with ammonia, extracted with ether, dried, and distd under reduced pressure.
Metzler and Tobolsky refluxed with only 10% (w/w) of acetic anhydride, then cooled and poured into excess 20% HCl, which, after cooling, was extracted with diethyl ether. (The amine hydrochloride, remains in the aqueous phase.) The HCl soln was cautiously made alkaline to phenolphthalein, and the amine layer was drawn off, dried over KOH and fractionally distd under reduced pressure, under nitrogen. Suitable drying agents for dimethylaniline include NaOH, BaO, CaSO4, and CaH2.
Other purification procedures include the formation of the picrate, prepared in *benzene soln and crystd to constant melting point, then decomposed with warm 10% NaOH and extracted into ether: the extract was washed with water, and distd under reduced pressure. The oxalate has also been used. The base has been fractionally crystd by partial freezing and also from aq 80% EtOH then from absolute EtOH. It has been distd from zinc dust, under nitrogen.
Prev:No record
Next:No record - 【Back】【Close 】【Print】【Add to favorite 】
-
Health and Chemical more >
-
Hot Products
- 146725-34-0 8-Azabicyclo[3.2.1]octane-2-carboxylicacid, 3-(3,4-dichlorophenyl)-, methyl ester, (1R,2S,3S,5S)-
- 64742-81-0 Kerosine (petroleum), hydrodesulfurized
- 19461-29-1 N-ALPHA-DANSYL-L-TRYPTOPHAN CYCLOHEXYLAMMONIUM SALT
- 261761-76-6 Perfluorocyclohexanecarbonyl bromide
- 3658-77-3 4-Hydroxy-2,5-dimethyl-3(2H)furanone
- 24312-00-3 Castalagin
- 5002-47-1 Decanoic acid,2-[4-[3-[2-(trifluoromethyl)-10H-phenothiazin-10-yl]propyl]-1-piperazinyl]ethylester
- 27247-96-7 Nitric acid,2-ethylhexyl ester
- 461-72-3 2,4-Imidazolidinedione
- 1002-69-3 1-Chlorodecane
- 7367-83-1 METHYL-CIS-4-DECENOATE
- 523-27-3 9,10-Dibromoanthracene