Jayko
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Synthesis of 2,4-pentadione
Hey guys,
Due to the fact that i wanted to make some nice complexes with acac but the Acetylacetone is completely impossible to buy besides sigma or others who
do not sell to private persons i want to make it my own.
There are two ways of making it.
(CH3CO)2O + CH3C(O)CH3 → CH3C(O)CH2C(O)CH3 catalysed with bf3 - wich is not really favourable because of the fact that its hard to handle and should
only be used unter inertgas
and the second method is:
NaOEt + EtO2CCH3 + CH3C(O)CH3 → NaCH3C(O)CHC(O)CH3 + 2 EtOH
NaCH3C(O)CHC(O)CH3 + HCl → CH3C(O)CH2C(O)CH3 + NaCl
this methode is much more preferable due to the fact that there are no such harsh chemicals like bf3 used.
Nontheless the sodium ethoxide wich is used here is also not buyable - or i just couldnt find any source that sells to a private person-.
So here is my question:
How can i make the sodium ethoxide myself or where can i buy it - preferable from ebay or something like that.
The only methode i found was to react sodium with ethanol....
even if this is a good methode could you please post some websites where i could buy chemicals ?
Thanks in advance
-Jayko
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j_sum1
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I bought some sodium from onyxmet.com, based on Poland. They are good.
Alternatively, you could make your own sodium. There is a recently developed method that brings high yield Na within the reach of amateur chemists
using OTC chemicals. It does however require high temperature stirring for 24 hours. Look for Nurdrage on YT.
Reacting NaOH with Mg turnings in a thermite-style reaction works. I have found the use of a cast-iron pot with a lid causes evaporated Na to
condense and solidify on the sides of the vessel in reasonable purity. You can scrape that off. Yield is crap. And there is plenty more sodium
mixed in with unreacted manesium and slag at the bottom of the vessel. Getting it out and separated is a pain but it can be done.
Then there is always electrolysis of the molten salt. There is a good thread here and the process is reliable. There is a bit of engineering
involved however before you start. If that does not phase you then it is probably the best method.
If your need is sodium ethoxide and you you need it promptly and you can handle a bit of impurity, then I would go the thermite route for the sake of
simplicity.
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Jayko
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wow thanks for the fast reply.
thanks i didnt knew about this methode. also thansk for sharing the website where i can aquire the jumpstart sodium for this.
Does anyone have other websites where i can buy chemicals as a private person. The only one i know is S3-Chemicals wich is like a miniture sigma for
private persons in europe.
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fusso
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But EtOAc will also self condense to form Et acetoacetate. How would you remove acetoacetate from acetylacetone?
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Jayko
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Quote: Originally posted by fusso  | | But EtOAc will also self condense to form Et acetoacetate. How would you remove acetoacetate from acetylacetone? |
Its no problem because the HAcac is deprotonised with koh to get acac in sito for bonding as chelate ligang to fe or other metals like cu.
Also the condensation is pretty slow as far as i can remember and takes weeks.
[Edited on 16-2-2019 by Jayko]
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clearly_not_atara
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I should point out that anhydrous NaOH can also be used to make NaOEt in amethod due to Organikum:
http://www.sciencemadness.org/talk/viewthread.php?tid=2656
Be aware that anhydrous NaOH is about as difficult to handle as Na itself, but it may be easier to make/obtain larger amounts. Always wear goggles
when handling it as the dust can burn your cornea.
[Edited on 04-20-1969 by clearly_not_atara]
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