mdp2p from oxone

[noj]

Will a duplicate hydrolysis/rearrangement harm ketone? Someone forgot to label a flask and was thinking of refluxing in 15% H2SO4 to make certain.

BTW, toluene is very ineffective as a substitute for DCM. In this instance anyway.
crucify the ego before it's far too late
and you will come to find that we are all one mind

[Rhodium]

Yes, running the acid hydrolysis twice as long, or two times in a row wil hurt yields.

[Vibrating_Lights]

Chromic,  what are your thaoughts on adding (aq)saturated oxone dropwise to alkene in meoh like with the modified peracid techniques.  earlier you said that there was no unreacted alkene just over oxidation products in the post rxn mix.  It seems that rxn would be less prone to side products if  full ammount of oxidiser was not present for the durtion of the rxn.
VL_

[Chromic]

The yields are already near 100% so I don't see how that would help improve anything...?

[noj]

Man I really like the outcome of this procedure. Someone had a strange accident in which while distilling the solvent out before vacuum distilling the ketone, the whole flask foamed over leaving someone with what ressembled foaming beer. Taking it back out and doing a few more basic washes and filtering the nasty emulsion... left someone with a very nice light yellow liquid. Well someone is distilling this none the less, and all is okay now. This could be a method for people without a vacuum to perform and see good results! If the ketone can be cleaned up so well with 4-5 basic washes, it may work out in an amalgam.
crucify the ego before it's far too late
and you will come to find that we are all one mind

[Chromic]

In addition, vacuum distillation is only necessary to see your true yields. I've distilled epoxide at atmospheric pressure (epoxides turn to ketones at high temperatures) and amalgamated and it was OK. I'm very sure it works with isosafrole (as I successfully did it with isosafrole epoxide as well... but never got high yields do to a messed up Al/Hg)... more experimentation is needed in that area.

[noj]

I've distilled epoxide at atmospheric pressure

Explain that... you didn't reflux for 2 hours as in thermal rearrangement? Simply distilling the epoxide resulted in ketone coming over? Man, someone is starting to see some very wet dreams ahead.
crucify the ego before it's far too late
and you will come to find that we are all one mind

[humidbeing]

Shit! Nothin like a little suspense!
excons make wonderfull employees

[Chromic]

Thermal rearrangement is heating the epoxide to about ~260C and holding for a few minutes, cranking the heat, and distilling it... it comes over somewhere around 300C (I didn't have a thermometer that went above 260C). What distills over is not epoxide, it is ketone. The crude yield is about 80%, the flask is relatively hard to clean afterwards. It has not been verified to give a good purity, but I know it works, and I think the purity is decent.

[humidbeing]

Bump!
 This is as interesting as it's likely to get right now!
" It's the smell!.......I feel saturated by it...

[noj]

If nothing comes over between the 260° and 300° mark, could it be that the epoxide is rearranged to ketone after a few minutes? All one would need is to let cool and distill under vacuum to yield perhaps 67% as V|_ mentioned with his thermal rearrangement. Guess someone will have to try this.
crucify the ego before it's far too late
and you will come to find that we are all one mind

[humidbeing]

Any results?
singel wite intejunt male

[noj]

I would, but the current setup limits me to 270°C.
Real men cook naked.

[cheeseboy]

cheese will try....cheese will try...cheese will try. Did cheese mention the cheese will try. OK
May The Source Bee With You....Always.

[humidbeing]

Good deal cheesy. Waiten!
Honey? Where's my little black medical book?

[uemura]

Chromic and all other bees...

Thermal rearrangement is heating the epoxide to about ~260C and holding for a few minutes,

Browsing thru the mail of the last three weeks, Uemura recognises that thermal rearrangement of epoxides is now an established method in the community

Now, there seem to bee a bit a confusion how long or if at all you have to reflux the epoxide. What uemura did was the following:

Put a high temp termomether inside the boiling liquid (use a 2-neck flask, 1 neck for the thermo, 1 for the condenser). Then watch the temp! In case of anethol epoxide you will recognise that boiling starts around 240DegC, then the temp climbs up slowly up to about 265DegC when it seizes at that level. Then add 5 minutes to complete the conversion. Replace the condenser by the usual destillation setup for normal pressure. The ketone Uemura got froze in the freezer.

Carpe Diem

[cheeseboy]

Failure....can you say "burned cheese"? Cheese will try again. Fascinating!

Cheese is using 100% OXONE from the hardware store. Sold under the label "Oxy-Clear" by DuPont. If DuPont makes it, it'sa the shit, no chlorine no nuthin' pure Oxone. $6.50 kg. The war IS over.
May The Source Bee With You....Always.

[sYnThOmAtIc]

Uemura,   None of the ketone pinky ever dealt with ever froze in the freezer though all his already had the nitro added with the proper nitro to ketone ratio ready for use in the al/hg. What is the mp for reference? Havent seen anyting but a bp.

Cheese,(or shoud I say COMPTON?) did yours fail in the epoxidation or the rearrangement?

[UKBEE]

You guys might find this useful ?

http://www.dupont.com/oxone/applications/index.html

I love the smell of Ketone in the morning.

[amalgum]

Uemura,   None of the ketone pinky ever dealt with ever froze in the freezer though all his already had the nitro added with the proper nitro to ketone ratio ready for use in the al/hg. What is the mp for reference? Havent seen anyting but a bp.

Well, the more diluted your ketone is in a solution, the lower the b.p. has to be for it to freeze.  Also, since you said you added nitro to your ketone, I assume your talking about MD-P2P.  Where as Uemura was talking about p-MeO-P2P made from anethole.