devongrrl
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Reference request
Does any one have access to the following article please ?
Vanillin Synthesis from 4-Hydroxybenzaldehyde
F. Taber , Shweta Patel , Travis M. Hambleton and Emma E. Winkel
J. Chem. Educ., 2007, 84 (7), p 1158
DOI: 10.1021/ed084p1158
Publication Date (Web): July 1, 2007
I haven't got access to References yet or I'd check there first.
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gsd
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make your reference requests in this thread
http://www.sciencemadness.org/talk/viewthread.php?tid=13196&...
gsd
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devongrrl
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If I was permitted access to that link, then maybe I would have.
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un0me2
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this one?... UTFSE, google to be precise....
PS It ain't a flame, but try it out - I personally spend a shitload of time on it, multi keyword searches, site specific searches, allinurl:, site:
etc. It is amazing how much is out there if you look.
[Edited on 9-8-2010 by un0me2]
Attachment: Taber.Patel.Hambleton.Vanillin.Synthesis.from.4.Hydroxybenzaldehyde.pdf (168kB)
This file has been downloaded 1517 times
quam temere in nosmet legem sancimus iniquam
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devongrrl
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Appreciate you pointing the pdf out to me, actually I do UTFSE a lot but I couldn't find that one.
Glad you weren't flaming me, I'd have had to use my CO2 extinguisher on ya 
The link gsd pointed me to lead me to:
"You are not authorised to view this forum"
hence my reply to him.
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mr.crow
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That paper is such a tease, it doesn't give the procedure.
You can ask a mod for access to the References forum.
Double, double toil and trouble; Fire burn, and caldron bubble
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un0me2
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Ummmm, it has the experimental procedure in the latter part of the 14 part file (the description thereof is at the start).
Running the reaction:
To the Br2-MeOH mixture in vial A, add 100 mg (0.82 mmol) of 4-hydroxybenzaldehyde,cap the vial and shake in ice-water bath for 30 seconds. Remove the
caps of both vials and pour the contents of vial A into the already-hot contents of vial B (Note 2). Replace the cap with the syringe barrel on vial B
and heat this mixture in the 130 oC silicon oil bath in a fume hood for one hour. During this time, prepare a flash chromatography column using 5.0 g
of flash silica gel. You should also prepare the solvent to be used in the column by combining 30 mL of Et2O and 170 mL of petroleum ether in a 250 mL
Erlynmeyer flask.
By the end of the hour, most of the solvent that was in vial B will have collected in the syringe barrel and a dark brown residue will remain in vial
B. Remove vial B from the heat source and let it stand until it is cool. Do not burn yourself! Remove the cap from vial B. Using a total of 6 mL of
3.0 M aqueous HCl and gently scraping the solid using a spatula, transfer the contents of vial B to a separatory funnel. Extract with 3x 5 mL EtOAc,
(a small separatory funnel or a centrifuge tube and a pipette may be used), combine the organic extracts and dry with Na2SO4. Transfer the supernatant
to a round-bottom flask, add 0.5 g silica gel and place the flask on a rotary
evaporator to remove excess solvent, leaving a dry light brown powder.
It then proceeds to deal with the preparation of a column and the subsequent chromatographic separation of the components. I wouldn't say that was a
"tease" as such...
quam temere in nosmet legem sancimus iniquam
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mr.crow
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Oh I see it now. WTF, why didn't I see it before?
Double, double toil and trouble; Fire burn, and caldron bubble
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