GreenD
National Hazard
Posts: 623
Registered: 30-3-2011
Member Is Offline
Mood: Not really high anymore
|
|
Dean Stark - Separating Acetone & Water? What?
"Investigations on heterogeneously catalysed condensations of glycerol to cyclic acetals"
The magnetically stirred (1000 rpm) reaction mixture (glyc-
erol, aldehyde or acetone, solvent, and catalyst) was refluxed in a 100-mLflask with a condenser. A Dean–Stark trap was
used to remove the formed water continuously.
They use the following reaction scheme:
Reaction mixture for the acetalisation of acetone: 0.1 mol glycerol, 0.15 mol acetone, 17.5 ml refluxing dichloromethane, 0.5 g Amberlyst-36 as
the catalyst. The given yield is related
to glycerol.
This is for the preparation of soketal
... Am I to assume that Water will form a layer, while acetone/DCM/soketal will form another?
Seems a bit odd to me, that removal of water is going to remove copious amounts of acetone... Make sense to anyone?
This seems to be the main reaction to produce soketal with the use of acetone.
ʃ Ψ*Ψ
Keepin' it real.
Check out my new collaborated site: MNMLimpact.com
|
|
|
Organikum
resurrected
Posts: 2337
Registered: 12-10-2002
Location: Europe
Member Is Offline
Mood: frustrated
|
|
Water removal by the DCM/water azeotropic system maybe?
|
|
|
GreenD
National Hazard
Posts: 623
Registered: 30-3-2011
Member Is Offline
Mood: Not really high anymore
|
|
Ran the expt verbatim, however only had a http://www.rightpricechemicals.com/media/catalog/product/cac... to separate water.
End up with dark nasty on the bottom, no separate layers on the top.
ʃ Ψ*Ψ
Keepin' it real.
Check out my new collaborated site: MNMLimpact.com
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
