Author Topic: o2 is the shit  (Read 20690 times)

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KrZ

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Post deleted by KrZ
« Reply #80 on: October 24, 2000, 09:09:00 AM »

zooligan

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Re: Frost is the shit
« Reply #81 on: October 24, 2000, 09:57:00 AM »

On a truly interesting note are those reactions using propylene glycol etc.  Now, if you aren't into those, which they say provide "total recovery of the catalyst system", they also mention another trick, extracting the post-reaction mix with DMSO to recover 50-75% of the catalyst system!


A retardo-ready-riteup (R3) describing this will make you even more of a hero than you already are K-man!  Especially with the prices and decreasing availability of PdCl2.


DiethylEtherMan

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Re: o2 is the shit
« Reply #82 on: October 24, 2000, 10:03:00 AM »
Dear KrZ:

 If you get a moment, could you post some links to some of the references you speak about. Something to get me going in the right direction. I have no idea where to find them online (or, if not online, where)?? Also, about the 'molar' form of measurment...I don't have the slightest clue about that. If you could post a link to a description of how to calculate molar weight to gram weight and how to calculate actual yeild percentages acccounding to molar weight I would be extremely grateful. Thanx again! I know, this newbee's a pain in the ass now. Sorry, guys!

This thread is getting better & better!

kpjr.

The reward of a thing well done, is to have done it well. Ralph Waldo Emerson

zooligan

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Re: o2 is the shit
« Reply #83 on: October 24, 2000, 10:16:00 AM »
Unobtanium posted a few links to some good molarity, molality, and concentration tutorial pages a while back, but that thread seems to have gotten clipped in the last pruning of the data tree (repost please, U-nob you).

Try this link for some basic chem concepts

http://pc65.frontier.osrhe.edu/hs/science/hchem2.htm



Mods, this question (and ones like it) seems to get asked a lot.  What happenned to LaBTop's sticky thread with all the educational links in it (I mean why is it not sticky anymore)?

z


CrystalDaddy

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Re: o2 is the shit
« Reply #84 on: October 24, 2000, 10:24:00 AM »
KrZ is a known liar as well as part time drugstore clerk.


KrZ

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Post deleted by KrZ
« Reply #85 on: October 24, 2000, 10:53:00 AM »

scram

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Re: o2 is the shit
« Reply #86 on: October 24, 2000, 01:40:00 PM »
LOL, I believe Frost. He's been speakin' to the man and getting good advise from him. Frost and I spoke about 5 months ago of which I traded alot of info on the sprayer method and said he was going to start doing it this summer. He got a source from me (if I still remember correctly) of which I thought the man would have already been aware of,  in which I would have traded that source with the an for some of this valuable information myself. If spiceboy claims 70% yields like mentioned earlier and being repeatable with just arm shaking, its not that much of a jump from 70 to 80% and luckily even 85% for a beginner. I'm beginning to think that ISA is a big factor of the high yields over MeOH.

Semtex

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Re: o2 is the shit
« Reply #87 on: October 24, 2000, 05:33:00 PM »
That may bee, but I believe that Osmium(feel free to correct me if I'm wrong) got good yeilds with MeOH(80%+...?) so it's not to say that MeOH isn't A good solvent for this rxn, but I do agree that from what the pimps are saying that IPA(what the hell is ISA? :P


::)  ::)

psychokitty

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Re: o2 is the shit
« Reply #88 on: October 24, 2000, 05:38:00 PM »
Epoxy paint is probably a much better coating material than teflon.  More resistant to weathering, that is.

--PK

Antibody2

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Re: o2 is the shit
« Reply #89 on: October 25, 2000, 06:16:00 AM »
Pychokitty - antibody has wondered about the viability of the epoxy coatings everyone is talking about. Acetone is a solvent that goes through epoxies like no tomorrow. Antibody assumed that ketone would have similar properties.

Scram -you missed my point, Didn’t say the wacker doesn’t run or that 80% is impossible, just that the way frost described it in 2.25hrs was what antibody had the problem with. Notice there hasn’t been a rebuttle from Frost.

Placebo - WTF, it never would have come to that if you weren’t asleep on the job, or moonlighting at totse or whereever.

KRZ - to extract catalysts into DMSO you would first need to get rid of your alcohol, right? DMSO is a polar solvent isn’t it?


Jimi loves ya

KrZ

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Post deleted by KrZ
« Reply #90 on: October 25, 2000, 07:52:00 AM »

Acme

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Re: o2 is the shit
« Reply #91 on: October 25, 2000, 08:09:00 PM »
IMO Frost is not full of shit.  Anyone who says he is, or KrZ too, dont have the sense God gave a mule.
I posit that the water, whatever it is doing, is not being incorporated into the product, that oxygen I am sure comes from O2

LaBTop

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Re: o2 is the shit
« Reply #92 on: October 25, 2000, 09:19:00 PM »
Last email received from a friend who isn't very fond of posting practical tests here:


-- I carefully fractionated the oil from the water-added O2 wacker and it's only isosafrole and a few ml's ketone.
The only thing I did different from KrZ's is : I used MeOH instead of IPA and shaker agitation.
Might try exactly one more trial using IPA and hand and shaker agitation just to be sure.
Really,  I'm just glad the benzo is almost here. --


For your info:
He allready checked out all possibilities mentioned in this thread from the first date of this thread and before that, and got very bad yields of ketone for the elevated (higher = 50 C) temperature O2-wacker,
then send me a very enthousiastic email about the results of the water-added O2-wacker, which was an oil, which he did the Frost-way, 2.5 hrs and KrZ's, 8 hrs,
then send me a pessimistic next one where he tried to aminate the oil with 4 different aminations, ALL shitty results.
And this was his last one.

He explained to me he did the Benzoquinone wacker many times before with a consistent >80% yield of ketone, and excellent aminations thereafter.

I don't think the IPA will give much or noticable better results, so it seems to be a very complicated way of making isosafrole from safrole.
 
It's a pitty, looked like a nice find, but as usual, the only real proof is amination and subsequently oral tests, in case you have no better techniques, like TLC, GC or NMR available. LT/



WISDOMwillWIN

Semtex

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Re: o2 is the shit
« Reply #93 on: October 25, 2000, 10:24:00 PM »
Are you saying that he tried an elevated temp wacker this time or prior to this time...?  I think the word around is that 55F not 55C was shown to give good results.  Other than that, I am not sure what the acual numbers are/were but I think Osmium's had some good exp with the MeOH/O2 wacker, maybe he could point out some hints/tips...?


::)  ::)

LaBTop

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Re: o2 is the shit
« Reply #94 on: October 25, 2000, 11:10:00 PM »
I'm re-reading his mails to find out if he used a glass or plastic vessel.
Osmium quote: Everybody knows that the product of the MeOH Wacker is the ketal, which is hydrolysed in a few seconds, maybe minutes afterwards as soon as you quench the reaction with acidic water. end quote.
Perhaps there could be a major mistake, but I doubt it, he mentioned quenching with the right amount of acid.
For your info: The elevated wacker was done in a warm water bath, before this thread.
This time he tried the Frost and KrZ methods, and both gave exactly the same results as them, O2 uptake measured :
Water added O2 trial O2 uptake fore each hour: 5, 4, 0. Rapid color changes.
No water added O2 trial, O2 uptake for each hour: 2, 4, n.a.(vessel breach), 5, 3, 3, 2, 2, 0.
So he worked with plastic vessels. Glas explodes, does'nt breach.
I still have hope.....LT/


WISDOMwillWIN

Antibody2

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rxn notes
« Reply #95 on: October 26, 2000, 06:52:00 AM »
Here are the notes that were kept during the rxn antibody discussed above (please note that an american thermometer was used during rxn)

1l heavy walled filterflask in a waterbath fixed with a 1.25" victor tire valve, was charged w/0.5g PdCl2, 2.5g CuCl2, 100ml 99%IPA, 2.5 " egg shaped stirbar. Stirred overnight.

9:30: flask  was charged with 50g safrole (0.28 moles), pressurized to 50psi, set stirrer on high, cooled bath from 61deg F->55deg F over 0.5hr

10:00: Stopped stirring, pressure had dropped to 40psi, opened flask charged with 3.5ml dH2O, resealed flask and repressurize to 50psi.

10:30: Pressure had dropped to 38psi bath temp had risen to 62Deg F, added two more ice cubes to bath, repressurize to 50psi.

11:10: Pressure had dropped to 43psi bath temp had risen to 66Deg F, added three more ice cubes to bath, repressurize to 50psi.

11:40: Pressure had dropped to 45psi bath temp had risen to 66Deg F, added three more ice cubes to bath(bath tempo dropped to 56F), repressurize to 50psi.

12:20:  Pressure had dropped to 44psi bath temp had risen to 64Deg F, added two more ice cubes to bath, repressurize to 50psi.

12:55: Pressure had dropped to 45psi. Stirring was stopped.

Total pressure drops 45psi or 3atm. In this flask with the reactants there remained 1.1litre headroom.
1l of Oxygen @1atm =1.42g
3.3l Oxygen @ 3atm =4.686g
0.2947moles of oxygen was consumed by reaction, a slight molar excess relative to safrole.

IPA was distilled at 45degC under medium vac, the remaining oil was passed through .25" 50mesh silica sand in a vacuum filtration set-up to recover catalyst.

Stirred filtrate with 200ml dH2O and 20ml 31% HCl for 15 minutes. Red oil that fell out was separated and the aqueous layer is extracted with 20ml DCM which is pooled w/ previous extract and placed in a 250ml rb flask in an oil bath, DCM is stripped off @ 760ttorr.

High Vac attached and applied
4mls of forerun are collected and discarded
30mls of safrole collected at 102-104 deg C
7mls ketone collected at 104-138 deg C
bit of polymerized crud in flask

Notes: the 2nd two fractions were tested with sodium metabisulfite 1ml each. The 3rd fraction crystallized immediately in the normal fashion, the 2nd fraction initially did nothing, but upon vigourous shaking finally began become turbid forming fluffy cystals over 1hour period at RT. (Crystals unlike any previously witnessed in similar rxns)

The 2nd fraction was reacted in a MM nitro Al/Hg, used the Ritter work-up, pregassed toulene was added to the washed and driied toulene extract until ph5 is reached. Nothing An hour later additional pregassed toulene added bringing PH down to 2 yield=0.0g+ONE PISSED OFF BEE >:(


Total time elapsed 11.5hours.

So there it is, flames welcome, Placebo?



Jimi loves ya

LaBTop

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Re: rxn notes
« Reply #96 on: October 26, 2000, 10:28:00 AM »
O2 is SHIT. LT/


WISDOMwillWIN

zooligan

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Re: rxn notes
« Reply #97 on: October 26, 2000, 11:01:00 AM »

O2 is SHIT. LT/



How eloquent.  Can you elaborate?

z


KrZ

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Post deleted by KrZ
« Reply #98 on: October 26, 2000, 11:09:00 AM »

Antibody2

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Re: rxn notes
« Reply #99 on: October 26, 2000, 11:51:00 AM »
KRZ, if its antibody you ask, he beleives the pressure of distillation to have been 5-10torr. 1st time this pump was used, so that is calculated by plotting the 2nd fractions BP on a nomagraph.

The pump was rated at 5millitorr ultimate vac , but it is not new. KRZ to be honest this was antibodies 1st crack at calculating mass of gases, so he fully expected after posting that to be told he had fucked up and calculated wrong.

The more he thinks about it, he wonders if the 2nd fraction was safrole at all, cause safrole doesn’t do shit with sodium bisulfite (antibody did a test tube worth of that too), so that part is confusing, because something, maybe traces of ketone reacted with the bisulfite from fraction2 yielding those very puffy crystals, some of them so weird they passwed through a cooffee filter. Is it possible the oxygen is bonding to another part of the safrole molecule?

Antibody is NO chemist (more a monkey who look at pictures, but cannot read) So where is all that O2 going? wish he knew. He doesn’t think there was a leak. If it were a leak perhaps O2 consumption would have been more uniform. IPA was used, you say that cannot be oxidized, so you tell me. Antibody is stumped, maybe a greater bee than me can solve this one.

BTW it was 50-65 Farenheit that was maintained.



Jimi is confused about this too