Author Topic: o2 is the shit  (Read 19450 times)

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frost

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o2 is the shit
« on: October 05, 2000, 03:10:00 PM »
fellow bees,
swinf would like to encourare the benzo loving bees to give the o2 wacker another look, swinf has had a few good o2 runs in the past but some that sucked and contained alot of iso. swinf with help finally has it down ands not looking back.
got a 40lb welding o2 cylinder with a 150psi self adjusting regulator = 170
used a 4ltr heavy walled filter flask this is awesome for adding the o2 with the clamp on hose
prestirred pdcl2 in denatured for 8 hours with a 3in eggbar
added cucl let stir for 1 hour, added olefin, put on rubber stopper strapped it down with plastic pullties, the strong kind, while friend put all his weight on the stopper then wrapped it up thouroughly with hose wrapping tape. 
added o2 up to 50 psi set the regulater, ran at room temp for 9-10 hours with high speed stirring.
the pressure dropped 12 times over this time frame the flask got very warm so obviously the exothermic reaction was doing its groove thing.
recommended ratios 1g pdcl2 to 5g of cucl to 100g olefin to 200ml of solvent. this one was scaled up, keep these ratios the same with the scale up.
ends up looking blackish with strong ketone smell,with no more pdcl2 being reabsorbed into the solution. hit with dh2o/hcl in sep, red ketone falls to the bottom, then wash water level with dcm to get what u missed, buchner through celite add to dcm/ketone, buchner again, looks greenish red now, strong ketone taste if ur brave enough to sample, when distilling little fore run then it comes over at pretty much the same temp, clear with a green tint,
very high yielding reaction, aminated some and boom u know what it did.
additionally,
using 2x solvent to safrole really helps to oxidise it much better with the hardstirring,was using too much before. no h2o was added.
thank you bees that have helped swinf work the bugs out of this. f-man, semetex, etc
frost over and out



PVnRT_NC8

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Re: o2 is the shit
« Reply #1 on: October 06, 2000, 10:03:00 PM »
??//


A010

FarQ

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Re: o2 is the shit
« Reply #2 on: October 06, 2000, 10:33:00 PM »
He wants to know what I want to know?
That is, what did you learn from him?


Stonium is a bitch, and yes, I love her.

scram

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Re: o2 is the shit
« Reply #3 on: October 08, 2000, 03:35:00 PM »
See man, told you this 02 tank shit is the bomb. For all of you cheap bee's flying with broken wings, you need to break down and put out the measly $70 for a 22cu ft 02 tank and $40 for a new regulator at Home Depot. All OTC, no names, no prescriptions needed for refills.
Frost,
How much actual ketone did you get from this reaction, how much actually aminated? I want to know because I have no glassware and have to guess/assume at my yields before the al/hg. Right now, got 250ml oil running in a reaction. Will let you know results soon.

KrZ

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Post deleted by KrZ
« Reply #4 on: October 08, 2000, 03:56:00 PM »

frost

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Re: o2 is the shit
« Reply #5 on: October 09, 2000, 01:52:00 AM »
KrZ,
did it in a room that the temp was 70f, the glass got very warm, have done it in ice bath but the yields sucked for swinf. how much longer should it go if done in a cooler enviroment, read on the old board the best yield u ever got was in a cold 55f room.so the longer the colder the better. sounds cool to swinf. remember you and os discussing the temp vs o2 absorbtion. love the o2 now, only getting a little whitish forerun before the goodies start flowing over.
thanks for the wisdom,
frost 8)  ;)

buchiguy

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Re: o2 is the shit
« Reply #6 on: October 12, 2000, 01:45:00 PM »
I read about this procedure on Rhodium a while ago from Spiceboy. I was wondering if anyone has tried using a paint shaker to get that major agitation that is needed to create oxidation? I was also wondering what would happen if we beefed the pressure up to 100 psi?\

 I also do NOT like the benzo/wacker because it uses a relatively hard to get, highly toxic substance, that creates a huge amount of difficult to dispose of waste. I can only get this stuff shipped by ground and it is kind of expensive, although the palladium is the real killer.

psychokitty

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Re: o2 is the shit
« Reply #7 on: October 12, 2000, 06:52:00 PM »
The only two times SWIM has tried this reaction with all reactants in the correct proportions was in the "bad-ass" soda-keg.  Both times a yellow oil was obtained that did not aminate and when put through several performic reactions, after dehydration of the intermediate, gave the desired ketone.  So, if one is interested in isoalkene, this is a good way to go.

My theory is that SWIMM's use of CuCl2 in this reaction was having a corrosive effect on the surrounding stainless steel.  KrZ has never reported this problem, so the only conclusion that I can draw is that he has either been lying all this time about the feasibility of this method (not likely) or his kegs are made of a type of stainless steel (possibly 440) that is absolutely resistant to corrosion.

SWIM is going to give this one another shot, but this time is going to coat inner sides of keg with epoxy paint, which is practically invulnerable to all solvents and reagents that it might be exposed to.

Comments?

--PK

KrZ

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Post deleted by KrZ
« Reply #8 on: October 12, 2000, 07:34:00 PM »

Semtex

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Re: o2 is the shit
« Reply #9 on: October 12, 2000, 07:57:00 PM »
I have to side with the KRZ kid on this one, I was in the thread that he speaks of...


::)  ::)

KrZ

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Post deleted by KrZ
« Reply #10 on: October 12, 2000, 08:07:00 PM »

zooligan

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Re: o2 is the shit
« Reply #11 on: October 13, 2000, 06:51:00 AM »

Not only that, I was the one saying it didn't work, citing journal ref's, and then getting suckered into wasting goodies on it 2 more times by some dildo who said it worked like a charm!



What doesn't work?  O2 in metal, 02 with this set of reactants, or O2 in general?


KrZ

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Post deleted by KrZ
« Reply #12 on: October 13, 2000, 08:36:00 AM »

frost

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Re: o2 is the shit
« Reply #13 on: October 13, 2000, 06:26:00 PM »
glass seems to be the way to go for most unless u can have a ss tank teflon coated the pdcl2 will react with anything else thats metal. as far as solvents meoh, denatured, ipa, even everclear or diesel all work but the best imho is lab grade etoh. ipa works well but for some reason it seems to work better with a little meoh, or etoh mixed in. that will help predissolve the pdcl2. everything but ipa labgrade etoh or everclear makes a blackish post reaction mix color itll be clearer and sometimes green with those. this thing works well especially at low 3atm pressure every time swinm tries to go high 60+ he starts to oxidise the solvent and the glass will get really hot using the 2:1:1:5
solvent to safrole to pdcl2 to cucl2 ratios. but with the lower pressures the ratios work every time with no tar or crap except for catalyst in the work up. the good vs bad ketone that hes seen always go like this if its very pure and strong itll be clear with a golden tint to it. all the bright green stuff that hes seen come from it looked like good benzo stuff does sometimes but it aminates poorly. resulting in crystals that when gassed look big and fluffy but when buchnered out are tiny, strange stuff man! but for swinf the clearish golden stuff always aminates perfectly with nice white xtals in high yield.
oh yeah dont try to pressurize those 4ltr filter flasks much over 45psi he saw one explode the other day at 65 psi thank god for tape! lots.....and lots. and that thing is fucking thick.
the best o2 container swinf can think of would be a pyrex media bottle with a screw on  top and have a glass blower attach a heavy duty vaccum pressure pyrex inlet like on the big f.f.'s for the 300psi welding air hose to clamp on to.


zooligan

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Re: o2 is the shit
« Reply #14 on: October 14, 2000, 10:17:00 AM »
What about PP or PE vessels?  One of those smaller water cooler bottles, perhaps? Or even a 3-litre soda bottle?  Will that material take the reaction?  It works in the SRV/KRV scenario...

z

terbium

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Re: o2 is the shit
« Reply #15 on: October 14, 2000, 10:33:00 AM »
I have gotten some pretty good explosions from reactions with high pressure oxygen. The O2 Wacker seems to be a good route but I wouldn't try to push the envelope with oxygen pressure - stay at no more than 1 to 3 atmospheres of oxygen. Glass vessels are good in a way, if there is an explosion then they will rupture at a relatively low pressure.

frost

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Re: o2 is the shit
« Reply #16 on: October 14, 2000, 11:00:00 AM »
ptfe vvessels or coke bottles will work if u have an orbital shaker but for magnetic stirring which swinf prefers with an eggbar it will wear a hole in it and cause a rupture. o2 is definately a viable route for oxidation. 45psi is enough for an 8-10 hour conversion, if using a glass vessel and highspeed eggbar stirring. also if using stirring make sure the bottom is wide enough so that when using 1:2 safrole to alcohol ratio you can see the bottom of the vessel while the eggbar is stirring this assures that all the mix is being exposed to the o2 for better, faster oxidation. start small like 100ml safrole in a 1ltre
filterflask the best way to cap one is to use a rubber buchner stopper with the small hole it fits flush with the top put a rubber cork in the hole that wont go through it and epoxy it in place wrap it with hose tape clamp on the o2 hose to the vaccum nipple and stir with a 3 inch eggbar for 8 -10 hours this works and works damn well, and you wont make a great big mess like with the benzo nonsense.
its not uncommon to get 85-90g mdp2p out of 100g of starting material and the work up is clean and takes no time
try either one of those with the benzo.
you can make ketone in no time and it will be very aminateable.
hope this helps
frost

Lino

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Re: o2 is the shit
« Reply #17 on: October 14, 2000, 12:26:00 PM »
Not dreamt the O2, but have been thinking about other pressure rxns and Zooligan's thoughts on PP/PE are valid. The garden sprayer could be the ideal low cost vessel of choice. It has a built in safety valve that blows @ 45psi, (could be tweeked higher maybe). The screw on top of the sprayers widely available where I live are easily modified to make a gas tight seal. Use a silicon bung (like the rubber ones from chem. suppliers) you fit it from the bottom of the screw on top so pressure helps the seal. Gas can be added via the threaded outlet for sprayer tube, or drill the silcone bung to accept a threaded adaptor for your T piece. The self tapping properties of the silicone bung should be adequate. The thickness of these garden sprayers should be safe at these pressures. Mag stirring is poss. if you somehow make the bottom of the spayer concave or flat. Maybe a resin soln dribbled in while rotating sprayer on a turntable to produce slight centrifugal force??? Whaddya think?

FarQ

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Re: o2 is the shit
« Reply #18 on: October 14, 2000, 12:39:00 PM »
I think the coke bottle with a tyre valve is the easiest safest way, there was talk on the old board of these things being capable of 100psi. So you would be relatively safe at 60psi. But one needs to be able to rig up something for serious agitation. I imagine getting a paint shaker would be difficult and expensive, but if you are good at making things, it shouldn't be that hard to rig up a small motor spinning an eccentic shaft for agitation.
Or you can always shake by hand, it has been done, but not by this bee, I wouldn't even attempt it. But making a shaker sounds like fun.

What size rxn would be possible in a 3L vessel (by safrole amount)?

frost

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Re: o2 is the shit
« Reply #19 on: October 14, 2000, 04:05:00 PM »
old frost has something that could possibly make the bees smile and flap their wings. the best of both worlds= one of the two harware store supersites has a galvanized steel tank that holds 2 gallons, and is epoxy coated thick epoxy called endurall tm. says its coated to with stand most chemicals and substances under pressure. its called the commando this made swinf think of all the cladestine acts he could accomplish with one of those. so you know he bought 2. btw clamped an o2 hose on 1's hose outlet and it holds 80psi easy!