mert
Hazard to Self
Posts: 80
Registered: 4-3-2006
Member Is Offline
Mood: No Mood
|
|
i have a problem..
what is Tos-Cl with crystallization? Which solvent? help please...!
|
|
|
falconZ
Harmless
Posts: 5
Registered: 4-1-2007
Member Is Offline
Mood: No Mood
|
|
toluene/pet. ether in the cold
----------------------------------------
p-Toluenesulfonyl chloride (tosyl chloride) [98-59-9] M 190.7, mp 67.5-68.5°, bp 138-139°/9mm, 146°/15mm, 167°/36mm.
Material that has been standing for a long time contains tosic acid and HCl. It is purified by dissolving (1Og) in the minimum volume of CHC13 (ca
25mL) filtered, and diluted with five volumes (i.e. 125mL) of pet ether (bp 30-60°) to precipitate impurities. The soln is filtered, clarified with
charcoal and concentrated to 4OmL by evaporation. Further evaporation to a very small volume gave 7g of white crystals which were analytically pure,
mp 67.5-68.5°. (The insoluble material was largely tosic acid and had mp 101-104°). [Pelletier Chem Ind (London) 1034 7955.] Also crystd from
toluene/pet ether in the cold, from pet ether (bp 40-60°) or benzene. Its soln in diethyl ether has been washed with aqueous 10% NaOH until
colourless, then dried and crystd by cooling in powdered Dry-ice. It has also been purified by dissolving in benzene, washing with aqueous 5% NaOH ,
then dried with K2Co3 or MgSO4 and distd under reduced pressure and can be sublimed at high vacuum [Ebel Chem Ber 60 20867927].
[Edited on 17-1-2007 by falconZ]
|
|
|
mert
Hazard to Self
Posts: 80
Registered: 4-3-2006
Member Is Offline
Mood: No Mood
|
|
a lot thanks falcon...
|
|
|
FANTOMAS
Harmless
Posts: 8
Registered: 23-1-2007
Location: Benthos
Member Is Offline
Mood: No Mood
|
|
to mert :
Please, when posting a new topic , be specific about it's contents .
Put the topic in the heading , and "I have a problem" in the posting .
That will help.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
