posted 01-08-2000 08:50 PM         

Somewhere I heard napthele talked about as the base precursor to another quinone?????.

This would be a classic,.

Thankyou

posted 01-14-2000 02:20 AM         

It was really goofing around with very little scientific method so its not really surprized that it was a total failure.

posted 01-17-2000 09:43 PM         

Maybee it's just the lack of a good strong proceedure, that stopping the o2 wacker from getting any where.

It is my gut feeling that pressurized O2, just isn't as good as the chemical family of the quinones,' in it's ability to consistently produce ketone,.

Maybee if we can make our own oTC pseudo quinone life will jus that bit easier.

Can we do it,
CHemhack ,have we got the technology, and for that matter , what is the final product which comes from the mothballs?.,
Have you got the theory.

hellman

posted 01-18-2000 02:58 PM         

Forgive me if this has been discussed before, but the question that pops up for me is: why don't people bubble the O2 into the solution as it's stirring instead of doing the balloon thang?

Seems like you'd saturate it a lot more efficiently.

It's all academic for me since I personally feel that the benzo wacker is the coolest thing since <insert cliche here>.

posted 01-19-2000 08:12 AM         

hellman- #1) The O2 method is NOT riddled with failure. It is one of the strongest, most ass kicking ketone generators ever...
The AIR method, in research and development, was riddled with failure, and then the O2 method was inconsistent, but minor variables
were nailed down that were responsible for the inconsistent reactions. Spice said that
ala Osmiums instructions, he discovered that predissolving was massively important.
Think about why benzoquinone works so well. Remember the posted improvements? Pre-dissolving is of the utmost importance.

#2) Napthalene, can, in theory, be oxidized to napthaquinone, which would be , basically, benzoquinone with another ring added to it. Alkenes are harder to oxidize than alcohols, etc, and the smell will send you running.

Methyl Man- It's because the O2 is more soluble under pressure, just like soda pop, w/ CO2. It goes flat @ atmospheric.

egotrip

posted 01-19-2000 10:44 AM         

As for oxidizing reagents, my personal favorite is good old H2O2. Cheap, effective, and requires no fancy equipment, and no headaches from worrying about two phase systems or anything else silly. Call me a pansy (actually, you'd better not call me a pansy, or I'll have your legs broken), but I've never felt entirely comfortable about combining pure oxygen, powerful oxidation catalysts, and highly flamable volatile solvents.

------------------
-the good reverend drone

Ipsa scientia potestas est

posted 01-19-2000 10:47 AM         

As for oxidizing reagents, my personal favorite is good old H2O2. Cheap, effective, and requires no fancy equipment, and no headaches from worrying about two phase systems or anything else silly. Call me a pansy (actually, you'd better not call me a pansy, or I'll have your legs broken), but I've never felt entirely comfortable about combining pressurized pure oxygen, a powerful oxidation catalyst, and a mixture of highly flamable volatile solvents on purpose. Yes, its "safe" but my "inner wuss" just remembers that 99% of the people here are not operating labs up to OSHA standards.

------------------
-the good reverend drone

Ipsa scientia potestas est

posted 01-19-2000 01:53 PM         

Predissolve 0.012 mol PdCl2 and 0.080 mol CuCl2.H2O in 300 ml MeOH and stir for approx. 12 hrs.
In a stainless steel pressure vessel combine the predissolved catalysts, 2.48 mol of terminal alkene and 1600 ml MeOH.
Start vigouros stirring (3" pear shaped mag.) and pressurize for 10-11 hrs with 75 psi of O2 (using a regulator to monitor pressure). When finished add 5 mol of H2O and stir for an hour (at reg. atmospheric pressure).
Yield of ketone after work up: 2.30 mol (93%)

The credit here goes to Osmium and Krz whose
wonderfull work turned me on to this one. It's so beautiful in its simplicity. But hey, you don't have to believe me. It's probably better that way. Hah hah.

posted 01-19-2000 06:04 PM         

Sorry bro,I didn't count the water molecules on the dihydrate. The general ratio used was 1gm PdCl2: 3.5gm CuCl2.2H20: 100ml olefin.
I also believe that you can get away with a lot less PdCl2 and CuCl2. Possibly even omitting the CuCl2, as the O2 would reoxidize
the palladium back.

IPA, EtOH, DMF were also tried as solvents. All of 'em working. Curiously,when IPA and DMF is used the absorbtion of O2 is a lot faster giving off a lot of heat in the first 4 hrs. Aim to keep the temp at 40C or so.

posted 01-19-2000 06:17 PM         

You're funny. I'll tell you what,if you ever make it to North America contact me at tripleneck@hushmail.com I'll have a 10L can of your favourite... Would that suffice?

posted 01-28-2000 04:48 AM         

Oh kids! If you get an old soda fire extinguisher(ss with 4" port and 500psi rating), regulators with 1000psi line pressure ablility(the thousands were the only ones that could run 500psi line pressure), and bad boy magnetic stirrer, you will bee as cool as pHas3d.

..and I thought the cornelius kegs were cool.

Any ss welders out there? MF charged me $75 an hr to put a fitting on the tank. Like im made of money or something...

And you have to use hydraulic lines for those pressures.

posted 01-28-2000 09:12 PM         

So lets try and seperate the theory from the actual finished crystal,.

As we all know, everybody can get something from the o2 wackeeeeer, but again as we all know, who really got the ketone,.
A roll call will be started again in this thread, so I urge all patients who did get CRYSTAL after the O2 wacker, to put their comments and suggestions on the line,.
Iw would be good to see the confidence grow, with this baby, and an exact procedure established,.
-if you were successful, we will need to know, such variables like....

1) pre disolved catalyst/not
2) time frame
3) psi
4) shaking strength
5) refilling intervals
6) basic ratio of pd/ketone/cucl2.h20

I beleive, having seen the power of methyl man's exact proceedure, which has nailed the ritter amalgam,
that maybee we could nail the O2 in much the same way.
Although to tell you the truth we must continue our work here on another quinone,.

Anybody got the time to manufacture napthaquinone, and give it a burl,.
Napthalene sure is cheap and OTC.

hellman.

posted 02-01-2000 04:21 AM         

I haven't got access to literature this hour of the night,

Is it alanine that we seek as the base precursor, if so, this is easy to make, and easy to purchase,.
'know the old route starting from benzene to nitrobenzene to alanine with fe amd hcl as the hard to get precursors,.

Does someone know the route of alanine to napthaquinone?????,

Come on we are so close to finishing all uncertainties.

posted 02-08-2000 06:38 PM         

I do mean analine, I remember just the other day discussing if this chemical was available to a local chemist, Unfortuanately it's not available OTC as far as I can see, yet,.

I will be back!
But even if we did start from benzene, who really wants to play with that or start that far behind,.

Times like these make you wonder if only formic acid could be properly S.G'd, so we could go on making our ketone to raise absolutely no suspicion at all.

hellman,.

Osmium,
Could you help me and other bees in a preperation of napthaquinone.
Ponder the implications for a while, it sure would be good dad!

posted 02-08-2000 07:18 PM         

Literature.

Quinones are cyclohaxadiendiones, but they are named as derivitives of aromatic systems; benzoquinone from benzene, napthaquinone from naptha....you get the point...!
Many quinones occur in nature(Yeah as does formic acid) especailly hydroxyquinones,

Here the list, but no reference from where in nature.

o-benzoquinone,p-benzoquinone,toluquinone,fumigatin,1,4-nathaquinone,1-2,napthaquinone,2,6-napthatquinone etc.

Preparation.

The only important method for the prep of quinones is the oxidation of aromatic hydroxy and amino compunds. Substituted phenols or anailine derivitives can be used with some oxidising agents.
For example, p-benzoquinone can be prepared by the oxisdation of benzene or aniline with a variety of oxidising agents, but it then goes on to say good luck if you can a find a prep not starting from hydraquinone.

So here my 2 cents,.

Is benzene hard to get, if it's relativly easy, then we may just be able to make our own p-benzo, without hydroquinone.

This leads me to think that napthaquione is just a fancy version of the ever so simple p-benzoquinone.

Let it be said that we need an otc synth for whichever is the simplest to prepare.

p-benzo or napthaquinone!!!!!.

hellman
'Just wetting the whistle'
proposed method 1
benzene+hno3=nitrobenzene
nitrobenzene+tin/fe/hcl=analine
analine+mystery oxisiser(kmno4?)=pbenzoquinone

proposed method 2-preferred.
benzene+mystery oxidiser=p-benzoquinone

hellman
Please keep in mind i have vogels book which covers in detail the route of benzene to analine....