Author Topic: O2 Wacker MDP3P Oxidation Details  (Read 2386 times)

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Sh0rtTerm

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O2 Wacker MDP3P Oxidation Details
« on: October 23, 2004, 03:19:00 PM »
Assuming 1Kg post o2 wacker “mostly” mdp2p, ready for distillation, is 15% mdp3p (roughly 150g or .84 mol.), how would a quality conscious bee go about removing it? Throw in 163g or .84 mol. K2CrO4 and stir?

Looking at

Post 438347

(Rhodium: "3-(3,4-Methylenedioxyphenyl)-propyl-methylamine", Newbee Forum)
hints at oxidation with potassium chromate or manganese dioxide. UTFSE yields no proposed or executed reaction details.

#1) Should bees use a molar equivalent of the oxidizer? Slight molar excess?

#2) Which oxidizer is the most forgiving and safest for bees? K2CrO4 cas#7789-00-6 mol wgt 194.17 or MnO2 cas#1313-13-9 mol wgt 86.94?

#3) How should bees carry out the oxidation? Add and stir? Predisolve oxidizer? Heat? How long?

Higher purity benefits everyone!

Snakebyte

  • Guest
details pls
« Reply #1 on: October 26, 2004, 10:45:00 AM »
Did Swist actually do this wacker yet?  If yes, what was his exact procedure and has it been aminated before?  My grandma as well as other bees have tried that wacker via Krz and Grouch several times without success.


Sh0rtTerm

  • Guest
It hasn´t been tried, yet...
« Reply #2 on: October 27, 2004, 03:28:00 PM »
There are a pile of refs that parallel the reaction with varied levels of success. I thought it would be worth a shot.

I noticed the hive problems. Posted wild variations in reaction times, reactant ratios, pressures and agitation methods didnt dampen my spirit.

Just to double check, so The Hive Collective is saying that dmf/o2, meoh/o2, ipa/o2, krv and osmium variations are all bullshit?

I seem to remember that PdCl2 doesnt disolve in ipa very well, which led me to question those posts. Mechanical stirring has never worked well for me in hydrogenations, so I had no problem believing the mag stirring failures.

Now SWIST was planning on running small scale dmf, ipa/meoh and meoh at 2 to 4 atm, monitoring o2 uptake, temp and tlc to get to the bottom of this. Was going to start with the ratios for the dmf wacker from rhods site by krz and grouch at 2.5atm. SWIST thinks they are using too much solvent and cucl2. SWIST was also going to run a 200ml meoh/1gPdCl2/5gCuCl2hyd starting at 3 atm and no heat for shits and giggles. SWIST was planning on also running meoh/ipa mixes.

If these have been unrepeatable, why are they on rhods site and here? What about the refs? Wacker oxidations are not new.

Snakebyte

  • Guest
Well, my grandma doesn't have any experience...
« Reply #3 on: October 28, 2004, 02:38:00 PM »
Well, my grandma doesn't have any experience with alcoholic wackers but she has tried DMF and DMSO with pure O2 up to 60 psi and shaking from a paint shaker.  Tried with both CuCl and CuCl2 and used distilled sassy.  Used photography grade PdCl2.  Followed Krz's and Grouch's procedure exactly and resulted in almost no oxygen uptake!  She's dying to get this wacker to work so please post your results.  PM me if u want any other details.


Sh0rtTerm

  • Guest
thanks for the heads up
« Reply #4 on: October 28, 2004, 09:05:00 PM »
I´m going to try some of the higher published cat to reactant ratios, now. A note I made has the molar ratios working out to 107.86g saf to 3.55g PdCl2 & 17.05g CuCl2hyd in alcohol. I´ll start with MeOH at 3atm no heat, and if that doesnt use o2, I´ll heat. If still no go, then vap and try another solvent till I get pissed. Might as well do something while the distillations are going.

I cant beleive that the hive is full circle back to alt.drug isosaf routes...

Perhaps I´ll mess with ptc fun!

Sh0rtTerm

  • Guest
Oh, one more...
« Reply #5 on: October 28, 2004, 09:29:00 PM »
Anybee tried cyclohexaamylose in this?

Snakebyte

  • Guest
no no, try this
« Reply #6 on: November 02, 2004, 11:10:00 AM »
Alcoholic wackers have been done in the past with various yeilds and from what swim remembers, the ones in MeOH weren't repeatable or very high yeilding for that matter.  If swim were to try this again he wouldn't waste his time doing the same runs many have done in the past. He would do 1 or both of these experiments:
1.try using polyethylene glycol(PEG) 400 as solvent as per

https://www.thevespiary.org/rhodium/Rhodium/pdf/wacker.peg.pdf


or
2.try cupric acetate as co-catalyst in AcNMe2 as solvent  

https://www.thevespiary.org/rhodium/Rhodium/pdf/wacker.o2.cupric.acetate.pdf