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All 7 posts Subject: O2 Wacker MDP3P Oxidation Details Please login to post Down

Sh0rtTerm
(Stranger)
10-23-04 22:19
No 537333
      O2 Wacker MDP3P Oxidation Details

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
(Hive Bee)
10-26-04 17:45
No 537934
User Picture       details pls

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.

The easiest way to control people? Make them believe they're free.

Sh0rtTerm
(Stranger)
10-27-04 22:28
No 538178
      It hasn´t been tried, yet...

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
(Hive Bee)
10-28-04 21:38
No 538363
User Picture       Well, my grandma doesn't have any experience...

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.

The easiest way to control people? Make them believe they're free.

Sh0rtTerm
(Stranger)
10-29-04 04:05
No 538440
      thanks for the heads up

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
(Stranger)
10-29-04 04:29
No 538443
      Oh, one more...

Anybee tried cyclohexaamylose in this?

Snakebyte
(Hive Bee)
11-02-04 19:10
No 539240
User Picture       no no, try this

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.rhodium.ws/pdf/wacker.peg.pdf
or
2.try cupric acetate as co-catalyst in AcNMe2 as solvent   https://www.rhodium.ws/pdf/wacker.o2.cupric.acetate.pdf

The easiest way to control people? Make them believe they're free.

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	All 7 posts		Subject: O2 Wacker MDP3P Oxidation Details		Please login to post		Down


		Sh0rtTerm (Stranger) 10-23-04 22:19 No 537333				O2 Wacker MDP3P Oxidation Details
						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 (Hive Bee) 10-26-04 17:45 No 537934				details pls
						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. The easiest way to control people? Make them believe they're free.



		Sh0rtTerm (Stranger) 10-27-04 22:28 No 538178				It hasn´t been tried, yet...
						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 (Hive Bee) 10-28-04 21:38 No 538363				Well, my grandma doesn't have any experience...
						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. The easiest way to control people? Make them believe they're free.



		Sh0rtTerm (Stranger) 10-29-04 04:05 No 538440				thanks for the heads up
						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 (Stranger) 10-29-04 04:29 No 538443				Oh, one more...
						Anybee tried cyclohexaamylose in this?



		Snakebyte (Hive Bee) 11-02-04 19:10 No 539240				no no, try this
						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.rhodium.ws/pdf/wacker.peg.pdf or 2.try cupric acetate as co-catalyst in AcNMe2 as solvent https://www.rhodium.ws/pdf/wacker.o2.cupric.acetate.pdf The easiest way to control people? Make them believe they're free.

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