Hi,

Just planing to make som other MDxx compounds after last sucess with MDMA ( Thanks Vespiary!!!
but there seems to be problems with ketone.
There is very little about ketone stability and what effects it on the net.
I just looked at my ketone batch and I am afraid something might go wrong!

Most interesting thing is that my first batch I ever did 3-4 months ago is still green,
viscous when frozen,has same smell and gives great MDMA yields,while batches I made few days ago and month ago turned
totally yellowish from original green colour and smell more like safrole than MDP-2-P.
No further synthesis were done with this new ketone since most chemicals are consumed now, but it will be done ASAP.
Also, feather like crystals were noticed at freezer temperatures in all batches.

Only difference I did in my first synthesis was that I made only two NaOH 10% washes,
while I did more washes (3-4) in late batches than changed appearance.
Xylene was used for the first batch that is still great and DCM and toluene for the latest batches.
I realize that pH and exposure to light(not factor in this cace) might change color of some organic chemicals,
but does anyone have any similar experience!?

Is there any known method or additive to keep ketone fresh for longer time(expect making some MDxx and freezing)!?
Quantitative tests on MDP-2-P are highly appreciated!

I know about bisulfite, and NaI seems to work even better, but this seems to be somehow messy and complicated...
Is there anything to just add in, like food preservatives are added or something like that!?

What might be cause of such behavior of ketone!?
(one batch stays OK, and other goes weird.)

Now you are screwing me arround...
You mean NaI and bisulfite!?
I know it can be used to make adduct,it is on Rhodium,but it is not case here,it is too dirty,labor intensive and results in impure ketone that needs further purification.
Many pople tend to have futher problems with this method...

Storage in freezer is great way for me,but I don't understand why older ketone is still same while newer one undergo rapid change!?
That is real problem here...what causes it,how to stop it and determine how bad it really is.

If there is some simple method to determine ketone contest and is it decomposing or just changing colour,just give me a link,I am sure I saw it somewhere but can't find it now.

I doubt i would ever succeed in making final product w/o critical thinking skills!
Open mind(other ways to get same thing) is what plunged me in this trouble in the first place!
You misunderstood mine problem, that is probably because of my inferior English grammar skills.
I understand basic scientific method, I am just asking for EXACT known causes of the
presented problem,so I can eliminate them one by one...

(Had similar problem with Al/Hg reductive amination, when most people said it can be done in EtOH
successfully with same method that involves MeOH, BULLS..T it CAN'T!
It inhibits amalgation,has too high b.p. and acts weird when NaOH is added. )

Of course, only reason why is it degrading is environment or pollution.
Excluding environment we are searching for pollution.

I used vacuum fraction distillation every time, and re-distilled ketone that started to spoil,
so only pollutant might be iso-olefin but it is spoiling again!
Now I am thinking that reason might be:
1) olefine-ketone auto-catalytic reaction
2) too many NaOH washes(but don't know why)

I find out that extractions done with DCM haw bigger tendency to spoil, my conclusion is that DCM doesn’t carry away   
water and basic water soluble crap like xylene does in lower fractions, purifying ketone form these before it reaches
higher temperatures of ketone b.p.(hence faster spoiling) Only part of DCM tends to distill under normal pressure and than It makes mixture
of all fractions at once in receiving flask if not heated really slowly under vacuum...

Toluene is much better but it sometimes starts to boil into receiving flask under high vacuum due the low b.p.
an than screw vacuum rig.

Xylene works perfectly for me.

Sure,I will do only 1-2 NaOH ashes in the future and use xylene if available, but I need to save ketone I got now so
this is reason why I ask help.

Problem is in chemicals, peracids are strictly watched here and hard to come by.
I accidentally come by 1l of 99% formic acid,but more steps,smelly and much longer procedure
putted mine interest out of this method. I must try it at least once...
Now when I have more PdCl2 than needed for industrial scale it is bitch to change method :-(
Unfortunately p-benzoquinone, hydroquinone become even harder to come by recently...
I am considering O2 gas as oxidants for wacker Wacker but have no idea haw to make non-magnetic pressurized apparatus
that can be mixed with magnetic stirrer and won't kill me!

OK,we determined that adduct is best way for storing ketone,will do in the future,thanks...
But is there simple qualitative or quantitative test for mpd-2-p like there is one for MDMA?!

It doesn't matter,I would make adduct same day,but this puzzles me...
How come can it be less stable with this method when there are less polutants in O2 Wacker than in p-benzo Wacker?
One of our members has(or at least had,can't connect right now ) wab-page with complete Wacker using O2,
yields are higher than those with p-benzo and I think that reaction must be much cleaner since there is no hydroquinone/quinohydrone crap left.
Yes,I know p-bezoquinone is more selective and keeps double bond of alkenes in place,but this is important only during reaction,not after it became something else in reaction,right?! Hydroquinone became totally unavailable here, like p-benzo was for years! Only problem I have with O2 Wacker is reaction flask,
really don't have idea what to use to withstand pressure and that can be stirred magnetically.

Will send you link of successful O2 Wacker with stirring when I find it.
It would be interesting to try potassium peroxymonosulfate in addition to sodium as source of oxygen
in Wacker oxidation, pity it is hard to find them here...

And about adduct, should KI work same as NaI!?
I mean this is all about I- anion or!?

Interesting...are yields higher than those with formic acid!?

Nice,thanks!

First method seems great,unfortunately it is only theoretical,do you know if anybody tried it actually!?

Never had problems with ketone stability made using the Wacker process. There is for sure something wrong in your procedure (probably distillation), since you have feathers-like crystal in your product. The ketone melting point is well below freezer temperature...That means you have a contaminant in your product, since it freezes at those temps.