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Metacelsus
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Thanks!
If I ever I get around to it (after finals, probably), I hope to do a more extensive writeup/compilation of my procedures in the Prepublication
section.
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aga
Forum Drunkard
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Excellent acceptance speech from the Winner.
Congratulations, Well done, and i look forward to the write-up.
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CuReUS
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here is a good article for reducing the time of the reaction .quite similar to what CC did
http://www.sciencedirect.com/science/article/pii/00404039950...
[Edited on 7-5-2015 by CuReUS]
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byko3y
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UHP-tungstate oxidizes amines into hydroxylamines, while secondary amines are rearranged to nitrones (just like here http://www.sciencedirect.com/science/article/pii/S0040402010... ).
In case of TEMP the resulting product will be a non-rearranged hydroxylamine.
And here's an article about oxidation to hydroxylamine http://onlinelibrary.wiley.com/doi/10.1002/adsc.200505018/ab...
[Edited on 7-5-2015 by byko3y]
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CuReUS
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in the search for alternate catalysts ,I found this patent where they use CO2.
http://www.google.com.ar/patents/US4247480
| Quote: | The foregoing and other objects of the present invention have been attained by oxidizing a tertiary amine with hydrogen peroxide in the presence
0.01-2% by weight based on the amine of carbon dioxide (CO2) in the presence or the absence of an improver selected from the group consisting of
ethylenediaminetetraacetic acid and its salts;
Suitable improvers include ethylenediaminetetraacetic acid and its salts, stanate such as sodium stanate; polyphosphates such as sodium pyrophosphate
and tripolyphosphate; salts of hydroxycarboxylic acid such as sodium citrate; salts of polycarboxylic acid such as sodium oxalic acid.
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another one uses flavin,peroxide and air for oxidation
http://pubs.acs.org/doi/abs/10.1021/jo980926d?journalCode=jo...
maybe flavin can be obtained from beef liver extract,but I am just guessing here
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CuReUS
National Hazard
Posts: 928
Registered: 9-9-2014
Member Is Offline
Mood: No Mood
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in the search for alternate catalysts ,I found this patent where they use CO2.
http://www.google.com.ar/patents/US4247480
| Quote: | The foregoing and other objects of the present invention have been attained by oxidizing a tertiary amine with hydrogen peroxide in the presence
0.01-2% by weight based on the amine of carbon dioxide (CO2) in the presence or the absence of an improver selected from the group consisting of
ethylenediaminetetraacetic acid and its salts;
Suitable improvers include ethylenediaminetetraacetic acid and its salts, stanate such as sodium stanate; polyphosphates such as sodium pyrophosphate
and tripolyphosphate; salts of hydroxycarboxylic acid such as sodium citrate; salts of polycarboxylic acid such as sodium oxalic acid.
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another one uses flavin,peroxide and air for oxidation
http://pubs.acs.org/doi/abs/10.1021/jo980926d?journalCode=jo...
maybe flavin can be obtained from beef liver extract,but I am just guessing here
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Metacelsus
International Hazard
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My writeup is up in Prepublications.
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smaerd
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Cheddite if you ever need bands to run faster on a column due to your fine mesh size I have a little trick. I stick a eye dropper or pasteur pipette
into a rubber stopper. I hook a hose to that stopper and then a 10mL syringe to the other end of the hose. I stick the rubber stopper into the column
and pump air in periodically (never pull back on the syringe remove it to refill the air). It helps me a good deal where flash is not available.
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Metacelsus
International Hazard
Posts: 2539
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Location: Boston, MA
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That's a pretty neat idea. I'll keep it in mind.
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