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Author Topic: Palladium Chloride and 02  (Read 600 times)

newbiechem

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Re: Palladium Chloride and 02
« Reply #20 on: August 23, 2011, 03:07:53 PM »
The KRV system will work with AIR instead of pure O2?
someone i know did it (with AIR) and try to purify with bisulfite, and gots lots of chicken fat crystal!
NOW, wonder if these crystals are mostly isosafrol (which will also crystalize on bisulfite correct?) or if its inded the ketone!
anyone please care to help?
apreciate
tnks

lugh

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Re: Palladium Chloride and 02
« Reply #21 on: August 23, 2011, 05:54:57 PM »
You need to start trying harder to understand organic chemistry:

http://127.0.0.1/talk/index.php/topic,1407.0/all.html

http://127.0.0.1/talk/index.php/topic,461

http://en.wikipedia.org/wiki/Sodium_bisulfite

and of course as has to be said to way too many newbees, use the fucking search engines  ::)  The end results from the effort applied 8)
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superlative

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Re: Palladium Chloride and 02
« Reply #22 on: December 04, 2011, 01:57:30 AM »
What about Ozone?

You can get or make corona discharge ozone generators that works nice and easy. Its a much stronger oxidizer than oxygen. Bite me if im wrong:)

What makes P-benzo the oxidizer of choice anyways for a wacker?



atara

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Re: Palladium Chloride and 02
« Reply #23 on: December 07, 2011, 10:44:50 PM »
Ozone will eat your alkene for breakfast, and your equipment for lunch. Bad idea.

Dr. Tox

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Re: Palladium Chloride and 02
« Reply #24 on: December 07, 2011, 11:45:48 PM »
The KRV sucks. It's blown up during shaking etc. Fuck that.

Maybe shaking with Raschig ring packed containers would be better.

IMO, it's not worth the bullshit. Hooray for Spiceboy if it works well for him but otherwise, no.
Alimentary, dear Watson; I had a gut feeling.

superlative

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Re: Palladium Chloride and 02
« Reply #25 on: December 10, 2011, 05:48:44 PM »
Quote from: atara on December 07, 2011, 10:44:50 PM
Ozone will eat your alkene for breakfast, and your equipment for lunch. Bad idea.

Please explain. Are you talking from experience?

atara

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Re: Palladium Chloride and 02
« Reply #26 on: January 18, 2012, 07:47:19 PM »
http://en.wikipedia.org/wiki/Ozonolysis

Ozone is highly reactive. It destroys alkenes on contact; in high concentrations, it can damage many materials which are normally considered inert, including many types of rubber.

http://www.ozoneapplications.com/info/ozone_compatible_materials.htm

lugh

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Re: Palladium Chloride and 02
« Reply #27 on: January 18, 2012, 08:19:27 PM »
Quote
Ozone is highly reactive. It destroys alkenes on contact;

That's certainly the case under some circumstances, but ozone can be used to oxidize alkenes to ketones under other conditions  ;)  This was well known to a few members of the Hive, but obviously not to most in Academia  :-X  The attached articles explain how this particular oxidation can be done  8)
« Last Edit: January 18, 2012, 08:34:31 PM by lugh »
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superlative

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Re: Palladium Chloride and 02
« Reply #28 on: January 19, 2012, 12:06:12 AM »
Pure Ozone is pretty harsh i guess, but in natural concentrations i guess it can be utilized with great results. Ozone generators of the tesla type can be used to ozonate drinking water. Its the corona discharge type. When members far more knowledgeable in Chem says its not usable i respect that. BUT without sounding ignorant people have had good results before and i think it needs a closer study. I think the whole wacker process needs another look(re-spect). The Performic/acidic route is stable but very low yielding imo. The benzo-route is nasty. the alkyl nitrite route is promising even though some say its a finicky dead end. The yields are great but at a high cost of catalyst. i tried to post on another forum to revive the discussion, but i think it came across as i was fishing for a spoonful so noone bothered to reply. Kudos! Shake for persevering. i wasnt around at the time to chime in, but i am now. As soon as the supply of olefin is in order and having access to a GC/MS i will get back on it. In the mean time i hope the old boys will give it another shot. go bees! go bees!

thanx for the zip, lugh:)

lugh

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Re: Palladium Chloride and 02
« Reply #29 on: January 19, 2012, 12:43:18 AM »
Wikipedia refers to the articles by Criegee and Brahan in their article about ozonolysis ;)  There are other olefins that will work well as far as testing purposes  8)
« Last Edit: January 19, 2012, 07:00:08 AM by lugh »
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newbiechem

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Re: Palladium Chloride and 02
« Reply #30 on: February 24, 2012, 10:12:31 PM »
could the oxidation with pdcl2/DMA at high pressure O2 could be perfom at a stainles steel vessel? or would need something like ptfe?

thanks.

Polonium

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Re: Palladium Chloride and 02
« Reply #31 on: February 27, 2012, 04:24:12 PM »
novicebrchem,

I have heard anecdotal reports about this reaction being preformed quite successfully in a standard 2 litre soft drink bottle IIRC.
I would recommend you contact 'shake' as he has some experience with this reaction.

Polonium

lugh

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Re: Palladium Chloride and 02
« Reply #32 on: February 27, 2012, 06:38:31 PM »
Quote
I would recommend you contact 'shake' as he has some experience with this reaction.

The revised thread from the Hive started by Spiceboy:

http://parazite.nn.fi/hiveboard/novel/000108557.html

and Rhodium's page:

http://www.erowid.org/archive/rhodium/chemistry/wacker.krv.html

Shake may be able to answer a question, but contacting spiceboy might bee far more informative  ;)  He's online elsewhere  8)

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lugh

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Re: Palladium Chloride and 02
« Reply #33 on: February 27, 2012, 08:48:38 PM »
Quote
could the oxidation with pdcl2/DMA at high pressure O2 could be perfom at a stainles steel vessel?

One should carefully read this rather informative Hive thread:

http://parazite.nn.fi/hiveboard/methods/000057481.html

which caused the original poster to lose credibility on the Hive and another well known member to delete most of their posts rather than deal with the fallout of their content  :-X  Almost all newbee's queries that are posted have all been answered already long ago, the end results from the effort applied  8)

Chemistry is our Covalent Bond

akcom

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Re: Palladium Chloride and 02
« Reply #34 on: March 08, 2012, 05:56:25 PM »
lugh, any idea why KrZ delete all his posts?

lugh

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Re: Palladium Chloride and 02
« Reply #35 on: March 08, 2012, 06:48:18 PM »
Quote
lugh, any idea why KrZ delete all his posts?

He deleted his posts because of the erroneous information in some of them  :-X  That incident was why the time for post editing was limited on the Hive  ;)  One should be skeptical about anything he claims   :P  Some are factual, some aren't  ::)  He's not the only person to act in this manner  :(  This fact about what's posted on these web sites should never bee ignored  8)
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akcom

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Re: Palladium Chloride and 02
« Reply #36 on: March 08, 2012, 11:25:59 PM »
Thats a shame.  I always thought KrZ was one of the more knowledgeable bees there.  Is there anyone other prolific posters one should be careful about?

lugh

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Re: Palladium Chloride and 02
« Reply #37 on: March 08, 2012, 11:50:31 PM »
Most of what KrZ posted on the Hive was probably factual, but in that thread he chimed in supporting Frost's rambling charade of claiming impossible yields with some references that didn't even exist   ::)  The Hive staff confronted him about this and he then deleted all of the posts in an attempt to maintain his credibility  :P  There's not much point in trying to make a list of suspects, what members need to realize is that any published articles from peer reviewed journals are rather reliable, while journals in which peer review isn't done are sometimes otherwise  :(  The spiceboy version of the wacker worked for a lot of Hive members, but some had trouble with it as always happens  :-X  Chemistry is both an art and a science 8)
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Shake

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Re: Palladium Chloride and 02
« Reply #38 on: May 01, 2012, 05:40:38 AM »
Quote from: newbiechem on February 24, 2012, 10:12:31 PM
could the oxidation with pdcl2/DMA at high pressure O2 could be perfom at a stainles steel vessel? or would need something like ptfe?

thanks.

no the PdCl2 reacts with the stainless

as for the ozone

bubbling ozone will make you a damn fine carboxyllic acid, or maybe aldehyde and there isnt much hope of getting a ketone out of it.. Without some sort of solvent or ligand to slow down the oxidation effects, youll end up with the acid.. alot cleaner than the jones reagent though!

you can get fish tank bubblers that bubbles ozone, also ozone is used in propper laboratorys for oxidations they have thier little portable ozone generators, by the time the ozone is free of the liquid its not ozone anymore it breaks down and reacts fast
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