cavgdad - 15-12-2004 at 09:03
anyone have a writup for this reaction?
Protium - 1-1-2005 at 02:22
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.
runlabrun - 1-1-2005 at 05:41
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 - 1-1-2005 at 10:58
Do you think the product would be good enough to make ecstacy from?
HRH_Prince_Charles - 1-1-2005 at 11:52
"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]
HNO3 - 1-1-2005 at 11:59
No.
Your royal highness
trilobite - 1-1-2005 at 16:28
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)
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