Shrinivas
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Separation of Guaiacol & P Methoxy Phenol
Hi Friends
I have a crude organic mass containing Guaiacol, Di Methoxy Phenol, HQ & P Methoxy Phenol. I wish to separate these components.
I have tried distillation (vacuum) but the organic mass is getting charred.
Looking for alternative suggestions to separate these fractions.
regards
Shrini
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bfesser
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Thread Moved
29-8-2013 at 06:34 |
Crowfjord
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If vacuum distillation is not working, chromatography is probably the only other other option. Crystallization would probably be a pain with such a
mixture.
How did this "crude organic mass" come about? Synthesis? If so what is the target compound? Maybe an alternative can be suggested with more
information.
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killer_lapin
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If they are insoluble or slightly soluble in water you could melt the mixture in neutral or slightly acidic water then let it cool slowly. Then they
should start to solidify accoring to their melting point.
Since their melting point are between 24C and 75 this procedure might be feasable.
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sonogashira
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It is probably being oxidized rather than charred, and probably looks more extensive than it is. What temperatures are they distilling at?
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Shrinivas
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Quote: Originally posted by Crowfjord  | If vacuum distillation is not working, chromatography is probably the only other other option. Crystallization would probably be a pain with such a
mixture.
How did this "crude organic mass" come about? Synthesis? If so what is the target compound? Maybe an alternative can be suggested with more
information. |
TARGET COMPOUND IS 4-METHOXY PHENOL BUT GUAIACOL ALSO GETS GENERATED DURING REACTION. I HAVE TRIED TO HYDROXYLATE THE ANISOLE WITH ZEOLITE CATALYST
USING H2O2 AS OXIDISING AGENT. MEDIUM IS LOW BOILING SOLVENT. SOLVENT GETS SEPARATED EASILY IN DISTILLATION. BUT THE ORGANIC MASS DOESNT.
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Shrinivas
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| Quote: Originally posted by killer_lapin | If they are insoluble or slightly soluble in water you could melt the mixture in neutral or slightly acidic water then let it cool slowly. Then they
should start to solidify accoring to their melting point.
Since their melting point are between 24C and 75 this procedure might be feasable. |
pH is acidic. Entire mass is mixture of aqueous and organic phase (but doesnt show separate layers, as it got emulsified. i tried your suggestion but
it doesnt work. nothing solidifies. please suggest
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Crowfjord
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You would be better off starting with hydroquinone using methanol and sulfuric acid, ala this thread. Oxidizing anisole will give 50% yield of the para-methoxy compound at best, where the stated method has pretty high yields and only
starting material to separate at the end.
[Edited on 4-9-2013 by Crowfjord]
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