Author Topic: o2 is the shit  (Read 20687 times)

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frost

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Re: o2 is the shit
« Reply #60 on: October 18, 2000, 10:46:00 PM »
As i read it the good yields you were getting were with the rossi g-reactor tm at 80psi and the only prob was only 1 kg could be processed at a time. Probs were with the ss. in the all o2 probs solved thread was where the carboy idea came up there were pics and everything.on that same you were suggesting the use of ipa at a cool temp in glass with less psi. and os was saying that ipa wasent a good idea since everyone was getting such good results with meoh, and the discussion went on to arguing about the temp thing with os,then pressure, and then about a page of flaming.
good thread though alot of momental o2 breakthrus came for the o2 with that thread. :-[
still peddaling
;D

frost

  • Guest
Re: o2 is the shit
« Reply #61 on: October 19, 2000, 01:13:00 AM »
o2 was done again on a small scale 100ml 99% ipa 50gm safrole 1/2pgcl2 2 1/2g cucl2 1n 1 liter filter flask.
pd, cucl ipa prestirred for 4 hours done in cool water bath 55-60f temp was monitered carefully. alkene was added, along with 2ml dh2o, had the old 12/12 highspeed plate back in action so stirring was faster this time. 2 hours 10 minutes later stirring was stopped when pdcl2 quit going back into solution. mix wasent black this time but reddish green much clearer and less viscous than before. work up was same except added hcl directly to mix first and stirred for 5 min, then h20 was added stirred then added to sep funnel extracted as usual. distilled an got 47g ketone which was aminated with nitro,via balchemist method(thanks pal) gassed with hcl yielding 45g xtals.
swinf was very impressed. only a 5 g loss from start up! the whole thing only took 16 hours!
damn this place rocks
time for the scale up! gonna have to break out the pyrex 10L media bottle for that one though. just came back from the glassblower with the heavy duty air inlet now.
stirplate helped alot imho with the speed of this reaction the thermolyne cimatec wasent fast enough!
side note just as krz said there was no exothermic reaction with the ipa.
frost out!   :)

Osmium

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Re: o2 is the shit
« Reply #62 on: October 19, 2000, 02:38:00 AM »
Wow frost! Good post! Only two hours of reaction time?!
Bee careful with that big bottle! They don't like pressure like the small ones do. Better pressure-test it in a safe location first! I'd rather buy a second stirrer and work with two batches, having them running all the time you are in the lab. 16h/2:10h= ~7 runs. 7*45g*2=~650g ketone per day. Make the reactions 30% bigger and you end up with close to a kilogram. What more do you want?

All I said back then was that MeOH is a better solvent than IPA accoring to the refs. But it seems like IPA works just as well if not better. Very cool.

Semtex

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Re: o2 is the shit
« Reply #63 on: October 19, 2000, 05:40:00 AM »
So frost, your maxing out your stirplates then?  At the highest setting(s)?  What is the RPM difference between the two(if there is one) or do you mean the magnet is stronger in one...?  Nice post, any MORE luck with that epoxy coated bastage yet...?  ::)


::)  ::)

KrZ

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Post deleted by KrZ
« Reply #64 on: October 19, 2000, 07:48:00 AM »

sassy_sucker

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Re: o2 is the shit
« Reply #65 on: October 19, 2000, 08:05:00 AM »
Frost: What happened to the commando idea?  Did you find a problem with it?  If so, what?  What made you decide to use the filter flask?

 -SS


how would you fuck me?

DiethylEtherMan

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Re: o2 is the shit
« Reply #66 on: October 22, 2000, 11:35:00 AM »
Hey guys. I know I am a newbee and shouldn't even be close to this thread, but I have to ask a few questions (and yes, I have done my research, but am still a little confused). I have been reading much from Strike's book TS II and I am interested in making MD-P2P from safrole via O2, Palladium Chloride and Cuprous Chloride.

1) Has Dimethylformamide been deleted from the process altogether? In it's place can we use IPA or MeOH now?

2) In Strike's book 26.5 g Palladium Chloride was used for 500 g safrole...has this amount been lessened to 2g per 200 g safrole?

3) Is it possible to use Palladium Acetate in an O2 Wacker? (but not the H202 and tert butyl alcohol method mention in TS II)

Thanx guys, in advance! Please, no flamming had enough of that shit. I have really spent like 6 months reading books on this, and have just recently begun my own experiences. So it's not like I am just some young punk trying to bug the shit out of all of you experienced people before I try and find the answers myself. So, plese bear with me. (I have posted these questions on the newbee forum a bit back, but no one seemed to answer them, so this is a repost, sort of) Thanx in advance. And I would like to say that Strike's book TS II is an incredible book. Without it I may have been lost for longer than I was. Here's to Strike, for an extremely informative and step by step book.

If ya wanna see the rainbow, ya got to be prepared to put up with the rain!

FarQ

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Re: o2 is the shit
« Reply #67 on: October 22, 2000, 11:56:00 AM »
All your answers are here, read and thou shall find.


ML<--Meth Loser

LaBTop

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Re: o2 is the shit
« Reply #68 on: October 22, 2000, 06:46:00 PM »
Let's try all to come up with ideas to scale this beautiful MF up, it would by far be a better method then the performic.
The only reason to choose for the performic is it's infinitely upscalable nature. But you are left with a LOT of waste. And this one has a far better yield, and nearly no waste.

Frost, I will try to write your researchings up for the masses, and put it up high there where it belongs in the "Detailed Methods for Non-Chemists", combined with all the neat stuff provided by KrZ, Osmium and Baalchemist.
Exellent thread, to say the least! Good old Hive feeling comming back again. LT/

PS1: anyone ever tried ultrasound transducers in this method? Eventually combined with slow stirring and a commercially available high pressure seal, or just the big-ass egg stirrbar. Ultrasound accelerated Brownian motion in the reactionmix will provide for optimal agitation, let's hope.

PS2: glasslined SS reactors, second hand, lay around all over the world, in any amount and size.
I saw a beautifull full Pyrex-glass roundbottom 150 liter high pressure device (~5cm diam. wall), with 1 Hp magnetic stirrer motor on top of the lid and a magnetic stirrer plate under the lid with a shaft+mixer attached (so no leaking possible), hung up in a cradle for easy decanting.
It was rated for 5 atm ! Used, but looked brandnew, prize: $ 1500 !


WISDOMwillWIN

DiethylEtherMan

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Re: o2 is the shit
« Reply #69 on: October 23, 2000, 12:53:00 AM »
Hey, guys...I know I am a newbee and I am just barley following you guys by the skin of my teeth, but I think I found a really cool sight (in the future for me) with plenty of glass linned SS vessels from 1L to 600L. As well as all the pressure flanges & stirrers that you guys may need. I hope this helps people. Have fun and good luck. Thanx for all the very informative posts.

You can't steal second base and keep one foot on first.

When a man succeeds, he does it spite of everybody, and not with the assistance of everybody. <-- Edgar Watson Howe

http://www.qvf.co.uk


Antibody2

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Frost is shit
« Reply #70 on: October 23, 2000, 12:32:00 PM »
Older bees - antibody is not doubting the viability of the O2 wacker, but is antibody really the only bee in this hive to smell some BS in this thread?

The really sad thing aboput it is Antibody imagines that a whole herd of newbees are right now running off to try and duplicate the horseshit that frost claimed to have done. Antibody is not talking through his hat here either, he triied a very controleed reaction almost exactly as frost described, it ran for 3.25 hours . It yielded 20% ketone 70% safrole the other 10% was lost through polymerization during distillation and in the 24inchs of glass (column and condenser).

Antibody knew better before he even started, but could not tolerate having to listen to crock of shit the FROST is spreading all over the hive. So it was rerun overthe weekend  and yields were NO WHERE near what frost claims. If anybee is interested antibody kept excrutiating notes of this one for just such an eventuality.

Anyone remember frost claiming 90% on another O2 wacker, or his claim to 90% mda  (not mdma) yield from NaBH4 (NO ONE HAS PULLED THAT OFF YET!), or his claims of outrageous yeilds of pseudonitrosites and in his description he was claiming to be using Sodium Nitrate in a synth calling for sodium NITRITE! Antibody has received numerous dumb assed questions via PM that give ly to his ignorance. he even claimed that DCM would work in the 2phase pseudonitrosite synth, and it is the BOTTOM LAYER.

In fact all Frost is is a fucking parrot, agood number of his posts is plagerized from somewhere else in the hive.

DEA must bee busting thier guts laughing as all the old respected bees of this this hive lend thier credibilty to this little bullshit artist and not even a very good one. Search through some of his posts, it is apparent to anyone with the capacity to reason. LabTop you don’t really fall for this do you? Os? KrZ? Semtex n Sunlight? Antibody was under the impression you guys had it togather. This is a sorry day for the hive.

Love the refs you guys put up here and alot of the discussion is valid. But christ jesus , be careful what you beleive. Bad eneough some bees posting nonsense without the hive elders validating it.

Has anyone else been able to duplicate Frost’s miracle? Think there is more dupe involved here than miracle. Antibody has $200 for anyone who can prove that he has.

Sorry to rain on this parade but antibody cannot go another day without screaming out FROST IS FULL OF SHIT! >:(


Jimi loves ya

buchiguy

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Re: Frost is shit
« Reply #71 on: October 23, 2000, 05:26:00 PM »
Hey man! Think your being a little hard on this guy! He's not the first Bee to claim good results with this wacker you know! This idea was brought to my attention quite a while ago with the so called "Spiceboy Reaction Vessel" and he claimed over 50% yields with just manual shaking and compressed air. It seems logical that pure O2 and automated shaking would provide much better results. Frost is not the first guy to use this idea and claim it is viable buddy, so just because YOU didn't get decent results doesn't mean that it doesn't work, only that YOU must have fucked something up! So why don't you try to be part of the solution and not the problem?

I don't think the DEA is laughing too hard at this one, far from it, as if this method can be perfected it presents a major achievement in MDP2P production and will be much more difficult to trace chems as these are almost entirely OTC.

So why don't you just publish your results from an objective point of view, not slamming something until you are absolutely certain it is wrong.

buchiguy

  • Guest
Re: o2 is the shit
« Reply #72 on: October 23, 2000, 05:28:00 PM »
I've been told by numerous experts that the H2O2 wacker does not work at all so I wouldn't waste any time with that Frost. It sounded like an excellent method but no one has been able to get it to work.

IMPORTANT QUESTION! Earlier in the thread we were talking about pressurizing pesticide sprayers, as they are almost entirely plastic, but I have not heard any success stories. This is the method SWIM will soon try but would like to know if people had any difficulties before SWIM goes ahead, as SWIM may just opt to get a soda keg teflon lined if this is the only way to go, as SWIM thinks glass vessels are a bad idea for larger scales.

scram

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Re: o2 is the shit
« Reply #73 on: October 23, 2000, 06:37:00 PM »
7.6 liter (2 gallon for US citizens) max pressure 50psi (don't go higher)
4.2 liter max pressure 60psi (possible to go up to 80 psi, but over 65psi prepare yourself for possible injury)
Best bubbling action w 4.2 liter is a total volume of 600-700ml
Best bubbling action w 7.6 liter is a total volume of 1100 to 1300ml
Its best to get a regulator that maxes out at 60psi, you can even set it so that it won't fall below a given psi. Use belt straps (hook type) to strap the vessel nicely around the stirrer. Use only egg shape stirbars of 62mm or longer. Purge twice before starting the reaction to maximize volume of 02.
I had one of the 7.6 liter explode on me due to a faulty regulator which had worked the prior time. As a result, the bitch must have pumped up to 80 psi before blowing with a shotgun like sound and certainly would have broke my leg had it been aimed there instead of the wall. The whole HDPE was ripped with a 1/4 meter tear going lenghtwise. From now on, I double up and make sure psi 60 doesn't show psi 10 using a secondary inline psi gauge. I will not be fucking with glass anymore. Im not smart enough and should have heeded KRZ's advise on using 'vacuum' type carboys instead of the typical $10 carboy. Pumped a 3 gallon up to 35 psi, no problem. Before pumping to 45 psi the carboy was place under a hugh furniture box because of fear the stopper would blow-out. Not realizing the situation was going to much worse than that, it was pumped to 45 psi and about 1 minute later KABOOOOM, loud as a shotgun, really loud. Blew the MF in hundreds of pieces with the largest piece no bigger than my hand. Fortunately, shards were pretty much constrained to th inside of the box. I'll leave the dangerous work to the big boys from now on. I notice that after it broke there were significant varying thicknesses of the carboy throughout.

Semtex

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Re: o2 is the shit
« Reply #74 on: October 23, 2000, 07:45:00 PM »
Well I guess Osmium's full of shit, and the KRZ kid too, damn, should have known better...  :o

FOR THE LOVE OF HONEY, where the hell did you get that rant?!?  Give us some rxn details of these complete failures you are talking about.  There are NUMEROUS bees, much more knowledgeable(sp?) than you or I that have had success with this rxn, I really don't see what the problem is with frost having done the same.  I remember back in the day when Osmium and Spiceboy were fine tuning the SRV, hell when SWIM tried it for the first time he got a 20-30% yeild, and that's with AiR and hand shaking for a couple of hours!!!  I would honestly have to say to all that if you give this method the chance it deserves, you won't be disapointed. <----  That's a PERIOD... ;)


::)  ::)

DiethylEtherMan

  • Guest
Re: o2 is the shit
« Reply #75 on: October 23, 2000, 09:05:00 PM »
Hey, New Bee, here again. Someone please F**kin' tell me that Antibody2 is not telling the truth. Becasue I have been studying all of FROSTS posts to the F'in T and was soon planning on sending my researchings to a friend so he could try the synth. Someone here...anyone....a rubtle for FROST?

Dear Anti-Body, no disrespect to you, but I hope to god your not too sure of what your saying. Don't let it be true, brotha. But if it is, I suppose I would want to know since I spent alot of time reseaching this method and aquiring many items.

More comments, please!

kpjr.

If some of us were not so far behind,
The rest of you would not be so far ahead!

KrZ

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Post deleted by KrZ
« Reply #76 on: October 24, 2000, 05:04:00 AM »

Antibody2

  • Guest
Frost is the shit
« Reply #77 on: October 24, 2000, 06:48:00 AM »
Antibody Did not say the O2 wacker does not run, It Does run! Antibody has gotten high from using this synth.
The BS antibody is talking about is the yield Frost is claiming.

Antibody dxoesn’t think s0omeone with the amount of experience the Frost has is going to go out and trip over a 90+% yield


distilled an got 47g ketone


Lets look at this staetment for a second. Didn’t KRZ say earlier that the theoretical yield for this baby is 92%. Yet here is frost claiming 96%. Did pixies give him that additional 4%, and what about losses during distillation and work-up. You lose an ml in your distilation flask, you lose an ml in your condenser, you loss an ml or two AT LEAST during work-up, some in the funnel, some in the sep funnel. There is usually a little polymerization, NO? To get a yield like frost is claiming taking standard work-up and distillation losses into account he would have probably needed a  yield in excess of 100%. Where does a bee get those? In his imagination, thats where.

There aren’t many kitchen chemists that have those kind of work-up skills, and as antibody knows from the PMs he has received from Frost, that he doesn’t fall into that category, Sorry!

Antibody knows that this synth can run, he isn’t discounting what KRZ and Osmium have said, NO Way. Nor is antibody trying to discount the entire thread, it has a ton of merit as antibody has already stated earlier in this thread.

[/quote]Awesome thread

Quote


Antibody will get the details at lunch and post them.





Jimi loves ya

KrZ

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Post deleted by KrZ
« Reply #78 on: October 24, 2000, 08:36:00 AM »

placebo

  • Guest
Re: Frost is the shit
« Reply #79 on: October 24, 2000, 08:56:00 AM »
Thankyou KrZ, I was going to say that's a weight yeild not molar.
Secondly, how bout Frost gives us a super duper write-up in incredible detail, so that all us retards can follow it and not fuck up like antibody :o j/k.
I am also sick of Frost's vague posts.
If it's that easy Frost, please take the time to make a detailed write-up.
Just think....
If you do, and it is so easy to follow that all the bees suddenly start producing MDP2P in good yeilds. I am pretty certain all your previous stories wil be forgotten, and you will be a hero to the masses forever!



Hi Honey, I'm home!