cavgdad
Harmless
Posts: 22
Registered: 27-4-2004
Member Is Offline
Mood: No Mood
|
|
hcl hydrolosis of isosafrol glycol
anyone have a writup for this reaction?
|
|
|
Protium
Harmless
Posts: 27
Registered: 25-12-2004
Location: Point Of Return (Subject To 15% Restocking Fee)
Member Is Offline
Mood: unenlightened
|
|
A glycol is two alcohol groups...
Acohol + Halic Acid --> alkyl halide + water
R-OH + HCl --> R-Cl + H20
A mineral acid like H2SO4 or H3PO4 should do the trick though.
It just depends on how you look at it...
|
|
|
runlabrun
Hazard to Others
Posts: 172
Registered: 4-12-2004
Member Is Offline
Mood: No Mood
|
|
arent you lucky there are some hive members around  have fun, this is OC's
writeup i saved to disk:
HCl hydrolysis:
Thanks to Chromic I have never needed to do a sulfuric acid hydrolysis. HCl is really golden. In a 2L flask, you will have to do 2 hydrolysis by
splitting the glycol in 2.
You need
435 grams glycol
540 ml MeOH
900 ml water
900 ml muriatic acid
So 270 ml MeOH and 450 ml water are combined and warmed to about 60 degrees. The glycol is added(217.5 grams) followed by 450 ml muriatic acid. Upon
acid addition the solution will turn a little pink/orange.
The solution is refluxed for 2.5 hours at about 80 degrees celcius. It will start to change color maybe 15 minutes after acid addition. You will see
oil starting to stream on the top as it is stirring. One hour in, you will definitely see globules of oil floating around and the solution is more
brown by now.
After 2.5 hours, cool down to room temp using a water bath to speed things up a bit. Place in sep funnel and sep off bottom layer. This is your oil,
its dark red/black. The top layer is orange. Add a litle and extract the top layer again. 2 times 100 ml dcm is more then plenty I believe.
This step is repeated twice if you dont have anything bigger then a 2L flask
Take your dcm/oil( combine both hydrolysis then wash) layer and wash it a couple of times with 5%NaOH. Be patient and make sure all the dcm is out.
This can take multiple sepp off/wait cycles. But if you want to increase your yield do so. Then wash with fresh water, followed by brine. You can then
dry it even more with epsom salts if you want.
Distill dcm. Start vacuum and distill off your ketone.
-rlr
|
|
|
JohnWW
International Hazard
Posts: 2849
Registered: 27-7-2004
Location: New Zealand
Member Is Offline
Mood: No Mood
|
|
Do you think the product would be good enough to make ecstacy from?
|
|
|
HRH_Prince_Charles
Hazard to Self
Posts: 92
Registered: 29-6-2004
Location: Clarence House, London
Member Is Offline
Mood: Bombastic
|
|
"Do you think the product would be good enough to make ecstacy from?"
Is George W Bush a chimp?
Does anyone have a copy of Tetrahedron Letters 43 (2002) 9307-9309 that this is based on? There was a pdf copy on Rhodium but I don't have it
anymore. I think the gist was that 4M HCl gave best yields of various acids and Chromic had good results with 5M HCl.
[Edited on 1-1-2005 by HRH_Prince_Charles]
Loather of monstrous carbuncles, lover of organic melons and servant girls.
|
|
|
HNO3
Hazard to Others
Posts: 211
Registered: 10-11-2004
Location: America
Member Is Offline
Mood: No Mood
|
|
No.
\"In the beginning, God...\" Wait a minute, God doesn\'t exist!!!!!!!!!! \"OK, in the beginning, ummm, hydrogen...\" Wait a minute, what about the
laws of thermodynamics? \"OK, in the beginning, ummm.....UMMMMM, what\'s left to choose from?
|
|
|
trilobite
Hazard to Others
Posts: 152
Registered: 25-2-2004
Location: The Palaeozoic Ocean
Member Is Offline
Mood: lonely
|
|
Your royal highness
Effect of various acids at different concentrations on the pinacol rearrangement, Tetrahedron Letters 43, 9307-9309 (2002).
Attachment: Tet_Lett_43_9307-9309_2002.pdf (119kB)
This file has been downloaded 1231 times
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
