Any Oxone Sucesses

[Vibrating_Lights]

Have there been any sucesses with the oxone method and if so how far can it be scaled up.

[Rhodium]

https://www.thevespiary.org/rhodium/Rhodium/chemistry/oxonemethod.txt

That's the method, the scaling up is your assignment.  

[riobard]

Rhodium, is the method posted in that link the same one mentioned in chromic and improv_chem's 'research' posted in another thread? I believe chromic tried it out on anethole, but i didn't read the thread from beginning to completion.
     I'll have to look up the reaction details in a greater depth first, but i can't see a reason not to try it out once familiarity has been established. Time to use "The Fucking Search Engine(i see it's copyright protected/restricted now   )" Are there any links or references about oxone mechanisms and the like?

[riobard]

Oops, if i had looked harder i would have seen the 2 Journal Org. Chem refs on the page. But are there any others?

[Chromic]

It works on anethole and isosafrole and produces pmp2p and mdp2p respectively. It works well as written. Go for it, you won't be disappointed in your ketone, and certainly not in your amine.      

[riobard]

Ok, once some material has been procured i'll get on it and see what happens. This is actually desriable because of the restrictions on GAA and formic acid around here. I was wondering how to circumvent that when i wandered into this thread. If i could get my hands on unwatched GAA i'd like to try that epoxidation reaction too since it's covered in entirety on this site. I like experimentation a lot actually, and money has never been a motivation of mine in this pursuit. I'm happier when i'm getting my hands dirty.  
     If it all goes well I'll surely post a write-up and then a bioassay after red-amination with coresponding yield information. Be a little patient though, I'm not exactly trying to draw attention to myself and i still have a few things to get. Since i don't sell product and don't intend to, I guess i at least have no snitches to worry about.

[improv_chem]

I would really like to see your results from amination of the distilled ketone.  SWIM's experiments were small scale and ketone wasn't distilled.  Even with messed up Al/Hg's SWIM got some product(not great yeilds form the AL/Hg) that blew me into orbit. 
Good luck!
-improv  
Let's play with nature a little, I'm sure we can make her a little higher....

[Chromic]

I only ever aminated ketone from the Oxone runs once (using the results of the last run), and I remember getting a few grams of mdma from the distilled ketone. I ran a very small scale MM nitro reduction and because I did such a poor workup (I had broken my sep funnel after extracting the epoxide) even if I did have such info it would be basically meaningless.

[riobard]

Things are coming together but SWIM is still waiting on an item or 2. I figured that I should run a projected synth by you ahead of time to see if anything is out of place. Sassafras will be distilled via fridge compressor, isomerized in KOH/CaO.
    After that the oxone reaction will be run according to the link to your write-up on rhodium's page. Will scaling this reaction 5x be a possibility in a 2L 3N RBF? The reagent's haven't been weighed and placed in the vessel(partly due to abscence of oxone), so we have no concept of how full it will get at those quantities. SWIM isn't too concerned with the amount, just achieving a working environment in the flask. If no experimental work has been done in determining a relationship in scaling:yield that could be done as well. That will take a little time to compile and complete though.
       After the oxone reaction h2SO4 will be used similarly to the common peracid route. The ketone will be vacuum distilled, since no bisulfite is readilly available(SWIM is a bit picky about product purification, insisting on fractional distillation. He does this with all of his solvents prior to use, and to all of his products prior to corresponding use).
     Amination will be done via Al/Hg MeAm. Nitromethane is OTC, but SWIM got lucky this week with a bit of 40% aqueous methylamine. I've read that only minor alterations have to be made to the contents(adding a litle non-iodized NaCl, restricting any other sources of water) and yields should still stay at an adequate level. In addition the reaction will be less exothermic, with obvious benefits in scalability. Am I correct in assuming this? I guess it should be noted that the aluminum source would be reynold's heavy duty foil, balled up into nuggets; and the Hg would come from mercuric nitrate(the most soluble salt of it in water....coincidence? perhaps... ). I can't see any fault in these alterations, but maybe someone with more experience would know what I don't.
    Well, that's the plan. Now it's all just a matter of making it work. I have a little time before everything will come together, and i just wanted to check if all of my shit is together.

[Chromic]

You might be able to get away with putting 50g of isosafrole into a 2L flask by reducing the water/methanol so it all fits. Everything seems fine in your substitutions, good luck and remember to report back.

[riobard]

Time to get a big ass beaker then

[Vibrating_Lights]

Home brew stores sell 8 gallon pyrex flasks for cheap. teehee

[zooligan]

Flasks?  Really?  Like with gg joints?  Or are you talking about the big carboys with the big wide neck?

That reminds me of a joke....

You've heard of the Mickey's Big Mouth alcoholic beverage.  do you know why the opening is so wide?  It's so they can get the horse's dick in there to fill them up...  

z
"And if we don't get some cool rules ourselves, pronto, then we'll just be bogus too!"

[RoundBottom]

i think they're talking carboys.  i have never seen one with a GG neck, but if you got a big rubber stopper for it and carefully sealed a claissen into it, then you'd be set. 

i've been thinking about this for a while, and i can't see any major stumbling blocks.  once you have 1 claissen, you can put a condenser, run a stir shaft through it, and an addition funnel on top of the condenser.  no room for a thermometer...   but then we all know it hovers at 64°C

[pimpmaster]

well in the brewing store i usually go to there are up to 40 liter pyrex flasks with gg joints. they sure would be tempting if one had enough precoursors.
they had rubber stoppers , im sure one could fit an condensor through a rubber stopper

[RoundBottom]

wow, if that's the case, then this opens up a whole new can o' worms.  what size joints are they?

[terbium]

flasks with gg joints. ... they had rubber stoppers , im sure one could fit an condensor through a rubber stopper
Flasks with ground glass joints fitted with rubber stoppers? Doesn't make sense. 

[Rhodium]

The oxone writeup in new clothes with new links:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/oxone.epoxidation.html

[sunlight]

With aq. methylamine 40 %, 100 grams of ketone in 800 ml of methanol, 100 ml of aq. methylamine and 50 gr. of activated Al. Reflux and yield is 75 %+, usually around 78 % best was 82 %. Depending, of course, on the purity of ketone.

[riobard]

Is that typically the best yield that most bees attain? I remember Osmium posting references of up to 90% from the aqueous solutions, but I'd have to look that up again to quote it directly. I guess it might be expecting a bit too much given SWIM's lack of experience performing the reaction. It's not exactly going to be amateur night out in the lab as there is a fair share of lab experience to go between us and a commesurate amount of background as well.
     Fuck it, we could stand to see c.80% yields anyway. It's not like it matters that much.  But getting the most out of this wouldn't be a bad thing...