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Author: Subject: Fétizon Reagent regeneration ?
DrMethyl
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[*] posted on 7-3-2016 at 05:02
Fétizon Reagent regeneration ?


Hello,

I prepared the Fétizon reagent for the oxidation of alcohol to ketone/aldehyde this way :

30 g of commercial Celite is stirred in 200 ml Ethanol with 20ml 37% HCl for 10 min, then filtered on Buchner and washed with tap water until pH is neutral. The activated celite is dried at 140°C overnight. The color changed from light grey to white.

32 g of AgNO3 is dissolved in 300ml water and activated Celite is added. Upon stirring, a solution of 1.2 eq K2CO3 in 200ml water is added dropwise. Ag2CO3 precipitate on Celite and the color turned to light green. The Celite is filtered again and washed with plenty of water and dried on a rotavapor at 80°C under high vaccuum. Toluene is added and rotavapored under vaccum to remove the traces of water by azeotrope.

Since Ag salt are quite expensive I would like to know whether its possible to regenerate the Fétizon reagent after oxidation. I have plenty of already used Fétizon.

Can I treat the dead Fétizon with conc. HNO3 and then add some carbonate in excess to precipitate again the Ag2CO3 ? Will HNO3 attack the Celite ? Will NOx trouble the making of new Fétizon ?

Thanks in advance,

Dr.Me

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Nicodem
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7-3-2016 at 08:36
aga
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[*] posted on 7-3-2016 at 12:40


Quote: Originally posted by DrMethyl  
I prepared the Fétizon reagent .... washed with tap water

Ignore this if you like, i know very little.

What i do know is that the words 'reagent' and 'tap water' are kind of mutually exclusive.
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clearly_not_atara
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[*] posted on 7-3-2016 at 17:17


Silver carbonate on celite (silica) probably won't be attacked by tap water.

Op: https://www.researchgate.net/publication/241248188_Procedure...

This should do the trick. You can't reactivate the silver, but you should be able to turn most of it back into AgNO3 and reuse it.

[Edited on 8-3-2016 by clearly_not_atara]
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CuReUS
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[*] posted on 8-3-2016 at 04:57


Quote: Originally posted by clearly_not_atara  
Silver carbonate on celite (silica) probably won't be attacked by tap water.

tap water contains Chloride ions ,which might react with the silver carbonate to precipitate it as silver chloride
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