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Steam dist. P2P?

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Author	Topic: Steam dist. P2P?
iudexk Hive Bee	posted 12-27-1999 07:58 AM Just a dream: P2nP is reduced to P2P w/Fe-HCl. The rxn mixture is then distilled and a whitish-cloudy distillate collects @95-100C, Fester sez P2P can bee steam distilled like this. Is this white oily liquid a bitch of a P2P-H2O emulsion or have I fuckd up? Many thanks, IudexK
Osmium PimpBee	posted 12-27-1999 09:57 AM No, you didn't fuck up. That's P2P. Can't you smell it?! But why an emulsion? It always separated cleanly when I did that.
iudexk Hive Bee	posted 12-27-1999 10:24 AM Thankyou Yep, I can smell it, but this is the first time I've made P2P , so I wasn't entirely sure what it smelt like. I dunno why it's an emulsion, but it is. I'll xtract w/DCM a few times and see what happen... Many thanks, IudexK
CHEMMAN Hive Bee	posted 12-27-1999 08:14 PM Sorry , but isnt this meth related ? I may seem bitchy , but where does one go on the hive to gain chemical knowledge( not how to make meth) I wanted to learn about polymers.Surely p2p is meth related too.My thread was closed . Dont get me wrong Rhoddium, I realise you have a job to do . and need to draw a line.I have a great deal of respect for all hive moderators.When one studies and searches for knowledge on chemical properties , isnt the chem forum the appropriate one to turn to ??? Sorry guys for interrupting your thread. Your topic is of interest to me also . I just felt I had to get this off my chest... I too will be experimenting with P2p synth soon.What is the appropriate forum.Meth or Chem??? Regards CHEMMAN
chemstu unregistered	posted 12-27-1999 10:10 PM FFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFFF
CHEMMAN Hive Bee	posted 12-27-1999 10:23 PM And now we have a nonsence poster.Has done so in several forums.Why not delete this imbecile ?Lets support fellow hivers .Or am I wrong ?
iudexk Hive Bee	posted 12-28-1999 08:49 AM CHEMMAN - I thought this post was more emulsion/separation (ie. chemistry) related than meth related. Also I almost never go to the meth forum because there's so much shit there. chemstu - Just fuck off. If you are still able to type in your password and log on to the hive, there is no xcuse for posting shit, especially not repeatedly.
CHEMMAN Hive Bee	posted 12-30-1999 07:05 AM Yea your right man .Ive just been very desperate and frustrated with a problem that I have now solved. Would fractioning help your cause.Havent checked relevent BPs though. Sorry Rhodium and all for little outburst. It just happens sometimes and people like Chemspu catalyse my bad reaction.
CHEMMAN Hive Bee	posted 12-30-1999 07:15 AM A thought. If acetone will go into a waterlayer, which we know it does.Then what are p2ps properties.I have yet to meet this sexy thing.Does the benzene rings presence make it much more non polar ??
iudexk Hive Bee	posted 12-30-1999 08:00 AM Methinks tis only slightly soluble in H2O
Linoleum Hive Bee	posted 12-30-1999 11:59 AM Hi Bees, The p2p (if it's there) will come over with the steam as v. fine droplets and will then accumulate in the recieving flask as a yellow oil floating on the water. (it can vary in color between v. pale and bright yellow I suspect with your starting material it would be a similar color to those crystals) Pour all into a large flask and add toluene or DCM to extract the oil. Separate in the usual way. Lino
CHEMMAN Hive Bee	posted 12-31-1999 06:46 AM If someone theoretically had PAA, and lead acetate.Is acetic anhydride needed, or is methyl group from the acetate.Pros and cons please.p2p yield etc...
Night Trojan Hive Bee	posted 01-01-2000 09:45 PM P2P can be distilled at atmospheric pressure (in the prescence of air) with little (or no/neglegible) decomposition (may smell somewhat burnt which masks the sweet smell but still works in the Leukart reaction). Vacuum distillation is probably recommended, though. Steam distillation is slow and may hydrolyze some compounds. I had an idea that P2P or similar higher boiling liquid (bp 200-300 C) could be distilled at atmospheric pressure while slowing flushing the apparatus with CO2 or N2 to prevent any possible oxidation (compare to tube furnace reactions for making ketones from carboxylic acids). Also, a centrifuge works good for seperating P2P emulsions (may depend on process used to make it, ie. byproducts, etc.)
Night Trojan Hive Bee	posted 01-01-2000 09:58 PM For PAA -> P2P, check out these tube furnace processes in the following references: US patents 2108156 2612524 2697729 2811559 3660491 3075016 4172097 4754074 5750795 Organic Synthesis Vol ? pgs 389-382 (methyl benzyl.......) (anybody know the volume #?). http://www.uspto.gov/
Botzwan~C7h7Ch Hive Bee	posted 01-01-2000 10:52 PM Oh I get it this aint p2p2 this is p2np phenyl 2 nitro propylene Iron is supposably used to reduce the simple stuff??? This would mean if I am following corectly???? That ya simply h2s04 some eph and that the nitro part is transfered to the hoydroxy position well in what solvent anyways???? So then not having the nitrogen at the two .............oh spot lbenzal ch-ch ..............h...nh2 Nitrogen was spent by adding something like sulph acid and then ya got h2s0-3 hooked up,,,of course water is given up and this exchange goes through the replacing of basic theft of the oh ggroup that has been bothersome, this would likely be done in still an acid solution Adding the fehcl iuron cloride??? Maybe but I think ussually that the iron mecuride is used its otc. The so4 this would likely be spent in such reaction? Anyways rust? So the ntrogen is alowed to saturate or replace the oxygen there as because of that the hs03- yep it made water of it would seem steal replaces w/ nirtogen there at benzc1 c2 whatever nomenclatur a use it dont mater I am a crypto anyways So adding the cloride spends the sulph stuff and the resultan tis that ya want likewise to hydrogenate the c1c2 however that there h2so??? is replacement is gots to be eiter o or cl this might be possible to at least some mechanism or decent yeild that might be seperable easilly, and as an added benifit could be one pot.... So that the nitro would in fact hop up to the right position that it once was occupying to begin with?? And when it left leaving the h there at if it had been hydrogenated SO that when n left leaving to be in acid thats making seence to me, um yea basic soluton woul proally not be a good idea I am at three but I hear that 7 is a posibility
Linoleum Hive Bee	posted 01-08-2000 11:28 AM FMAN, we now know who you really are. GOTO the couch, you'll see.
Night Trojan Hive Bee	posted 01-08-2000 02:29 PM Organic Synthesis Collective Volume II.
Xaja Hive Bee	posted 01-08-2000 09:12 PM For making P2P from PAA: Use PAA, Acetic Anhydride and Sodium Acetate. Easier and yields are better then tube furnaces and lead acetate methods. Search - plenty of info if search engine will let you find it. Ratios something like: 2:1:4 PAA:NaOAc:AA
Night Trojan Hive Bee	posted 01-09-2000 11:55 AM Check the patents and the Organic Synthesis article for the yields (they're high). If you don't use enough acetic anhydride (AA) in the PAA AA Na acetate reaction you get a lot of dibenzyl ketone.
Night Trojan Hive Bee	posted 01-09-2000 12:06 PM In J. Gen. Chem. (USSR) 11, 339 (1941) in table I they show the yield of ketone using different proportions of PAA and AA. Their best yield is about 51% using 10 times the amount of AA compared to PAA. You have to remove the excess AA after the reaction too.
Xaja Hive Bee	posted 01-09-2000 04:32 PM Somebee (Os, I think) claimed to get up to 70-80% yields. It is true that yields are traditionally 50% in this rxn. But lower with Pb acetate. But PAA/AA easier for average bee than tube furnaces. So if you can get tube furnaces happening, then cool. If you can't, then PAA/AA may be way to go.
Night Trojan Hive Bee	posted 01-09-2000 07:05 PM Use a silica or ceramic combustion tube wrapped with a heating tape and glass wool for the tube furnace. Its a lot easier than seperating the ketone from excess acetic anhydride and Na acetate. You can get acetic acid OTC from some photo supply stores. Acetic anhydride is watched and not OTC. What comes out of the tube furnace is an organic layer on top of a water layer. Wash with NaHCO3 solution and use a centrifuge to seperate the emulsion. If you distil the organic layer at atmospheric pressure, most of it distils in a narrow range with the bp about where P2P distils. This works even without using an organic solvent for extraction. The product comes out of the tube furnace as a light yellow liquid, smells sweet and works in the Leukart reaction.
Xaja Hive Bee	posted 01-10-2000 12:01 AM Thought those furnaces had to be stuffed full of thorium oxide?
Night Trojan Hive Bee	posted 01-10-2000 08:28 PM Check the patents. They use other catalysts. You can look at the last three at http://www.uspto.gov/
Xaja Hive Bee	posted 01-10-2000 11:02 PM Thanx. Will do.
CHEMMAN Hive Bee	posted 01-11-2000 04:53 AM Yes that is correct , or so Vogel tells me . I have a lot more interest in benzaldehyde and nitroethane to p2np etc.
CHEMMAN Hive Bee	posted 01-11-2000 04:56 AM Indecision has clouded my vision but I am now starting to focus.

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