I had posted in this spot during a few hours a much too lengthy angry answer, but have deleted it, it's not good to answer in rage.
So I'll keep it instead to a shorter, a bit more decent and calmer reaction:
Post 171271 (missing)
(LaBTop: "Successfull DMF O2 Wacker", Methods Discourse) :
""
This is you talking.""
NO, it's clearly NOT me, it's Grouch's voice and later in that thread KrZ's voice, (see text of DMF/O2 wacker on Rhodium), and I stated clearly that the text from Grouch was emailed to me.
Grouch sadly enough is since last year in prison, as we all know, and I don't know if he's still there. Is his friend still reading here, could he give an update please on his status?
""
the DMF/O2 wacker on Rhodiums page. And yes, it is inaccurate. I do not know what kind of stirring you are using,""
"" I also used a 3 inch stirbar and a Thermoline heavy duty stirrer that's rated to stir up to 132 litres."" That you can and have read in the same post, you seem to be selectively blinded and don't want to read what doesn't fit your conspiracy theories!
That's a VERY HEAVY magnetic stirrer, Grouch also told in the same thread that he had an O2 uptake drop because he didn't put the stirrer-setting back in the original highspeed setting after one of his O2-repressuring steps.
Grouch and KrZ both do not mention anywhere external heating of the vessel to 50°Celsius. Only exothermic internal heating.
But still they could aminate their ketone successfully, while you couldn't.
So WHO's inaccurate???
""
but for this reaction to be over in 200 min you must have the product to catalyst ratios that are much higher than the ones listed.""
I strongly believe you are constantly switching between data for a DMF and an alcoholic O2-wacker.
I do not believe that KrZ and Grouch were both mistaken (see their posting history), while you would be right, you talk again about a DMF wacker, that one works as announced by 2 trusted members.
""
And on Rhodiums page for that procedure you have a boiling point of MDP2P 114C. When the reality is that the B.P. of MDP2P @ 2mm Hg is 132C.""
THIS SEEMS TO BE THE HEART OF YOUR "PROBLEM", so listen carefully:
That "you" is not me, that's
KrZ, the one you trusted so much you start PMing him about this procedure!!! Now YOU in fact call HIM a lier, he won't be pleased eather, believe me.
""KrZ: Vacuum distilled at ~2.0 mm Hg to recover 311.22g PiperonylMethylKetone (MDP2P) fraction between 105-114°C. There was an Isosafrole forerun, and a minimal high boilingpoint and thus polymerysized glop after 114C."" He then AMINATED his product! He also sound as if he was professionally knowing his tools, and wrote down the data collected precisely!
If you should have some grey mass left over up there, you should start to doubt your OWN vacuum meter, method, vacuumpump , thermometer, and especially your whole fuckin attitude first, before accusing others!
You DID NOT MAKE ANY MDP2P TO BEGIN WITH, you admitted that you could not aminate any products, so how the hell do you have the guts to doubt those figures, based on some fuckin ALDEHYDE or whatever you made there instead of a ketone, and then start accusing me and about everybody here of misleading people???
You really seem to be on a "nailing" binge aimed at me (and even my colleagues!) without thoroughly checking your own "facts", so you start telling me for a change what triggered this behavior?
WHAT IS
YOUR PROBLEM??? I don't have one.
""
The truth is you have to run the reaction until the O2 absorbtion is over. That time will vary depending on the efficiency of your stirring. If you prestir the catalyst for 12-24 hours the yields are much better, 90% instead of 70%, but the reaction will not get hot on it's own with prestirring. You will have to apply external heat to 50C. Now tell me I am wrong! And I know all of you admins know that by heart, but you choose to mislead. Why?
https://www.thevespiary.org/rhodium/Rhodium/chemistry/dmfo2wacker.html
- for those who are interested.""
You have to heat an ALCOHOLIC wacker, however you don't have to but CAN add some heat to a professionally proceeded DMF/O2 wacker. As said weeks ago ALREADY. See:
Post 171802 (missing)
(Antibody2: "Re: my exploited private email", Methods Discourse), where we talked then about non DMF wackers. That includes alcoholic ones too, you know.
You keep beating a dead horse.
Btw, do you start to realize the stupidity of your own above statements? :
You did NOT succeed to aminize your "ketone", but still use all collected data from that FAILED test (nr 434171, you haven't posted any data of a SUCCEEDED one!) to try to tackle our COLLECTIVE knowledge? Are you INSANE perhaps??? In that case, get professional help.
The consensus here seems to be that the bp of MDP2P at 760 mm Hg is 187 celsius, and not 164. So your famous "25 degrees difference" remark, thrown out in obvious anger, I still don't get. I linked those posts with discussion about MDP2P bp's LATER, so what the hell was that hickup aimed at that day? You talk to yourself mainly? And that mirrors itself into your posts, leaving us with no clue what the hell you mean?
Learn to type comprehensive texts for others to understand, try to get out of your daily egoistic reasoning, and try to see through the eye of the reader when you proofread (if ever) one of your own posts before clicking Submit.
""
And you have the nerve to say: a cook that I trust, e-mailed it to me. What is your problem? Perhaps you can explain to me your motivation for this, you, Rhodium, the rest of you admins.""
Are you slowly seeing your own unscientific way of reasoning yet?
You in fact attack KrZ.
And then YOU HAVE THE NERVE to attack us? GO FIGURE!!!
NOTES for people with more logic:1. See
Post 436217
(Bubbleplate: "Well....", Methods Discourse) for a sudden yield increase with GOOD highgrade PdCl2.
2.
Post 171639 (missing)
(pmpB_4: "Re: my exploited private email", Methods Discourse) :
""
most asssholes(sp! 
) here that bitched about the IPA (LT/: an alcohol)-02 Wacker only fucked up because they didn't have the H20 in the IPA/PdCl2/CuCl2 prestir. They added it during the oxidation, and it was my fault their PdCl2 didn't solvate! Go figure!! ""
Osmium told in this thread (nr 439327) to add no water in the first IPA post of this thread, is this (old)statement above (2.) right or wrong for any ALCOHOLIC wacker, so also a failed METHANOL wacker as used by ARGON in nr 434171 where he added the water after the prestirring ??
And if right, thus his PdCl2 did not solute totally perhaps, another cause of the failure perhaps?
If he (2.) was right, then the alc.wacker prestirr could be much shorter with the water added?
In the DMF/O2 wacker Grouch and KrZ added also water in the prestirr (much more related to the safrole btw). So if one changes only the solvent, Methanol for DMF, why would there be a difference?
3. Wacker success, good and fast O2 uptake, depends mainly on HEAVY stirring, yes, got it at last? Heavy SHAKING is even better, much better gas to fluid contact.
It seems clear by now that ARGON did not heat that METHANOL wacker, so that will have been the main reason of failure in his post nr 434171.
Why the fuck he then starts rambling on and on about a well eshtablished (by many members) DMF/O2 wacker is still beyond my comprehension.
Is some mexican thug standing perhaps behind you with a machete, which he will carve in you when you don't succeed?? That's the way it starts to sound.
In that case, get out fast and start over again in a safer place. LT/
