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Author Topic: Re; Hydroxylamine  (Read 757 times)

reDEEMed

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Re: Re; Hydroxylamine
« Reply #20 on: August 13, 2011, 07:18:31 PM »
Quote from: overunity33 on August 13, 2011, 06:09:16 PM
Do your reactions make your body sore?
I wish. The shit I do is like a kid playing with fucking play-doh, totally elementary and beginner style. I know you know what I'm saying, you're overthinking my ribbing is all.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
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reDEEMed

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Re: Re; Hydroxylamine
« Reply #21 on: September 21, 2011, 05:28:53 PM »
Since this thread got totally derailed and stayed on topic, I feel the need to pull it somewhat off topic.

Hypnos, what of the procedure you posted in the original post? Does it work? I can't for the life of me figure out how simply mixing morphine with hydroxylamine would produce a HCl salt. Is this because it's assumed that you are starting with a HCl salt? If you're sourcing your morphine from pills it's prolly gonna be the sulfate. What if you use freebase? I can't see it working anyway, period. How does hydroxylamine acetalate something? Maybe I'm misunderstanding something, that is always a possibility. Who told you this and have you tried it?
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

hypnos

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Re: Re; Hydroxylamine
« Reply #22 on: September 22, 2011, 11:22:16 AM »
man I just wrote a Big post and in reply and its fuckt off to cyberspace!!!

I'll try again tomorow....I cant seem to pm anyone??? strange



Hyppy
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hypnos

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Re: Re; Hydroxylamine
« Reply #23 on: September 22, 2011, 11:24:29 AM »
 but in a nut shell in answer to your Q the Dream is of starting with a Hcl salt form of the M

laters hyppy
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reDEEMed

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Re: Re; Hydroxylamine
« Reply #24 on: September 22, 2011, 01:27:31 PM »
How about hydroxylamine acetalating someyhing? Does it work?
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
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hypnos

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Re: Re; Hydroxylamine
« Reply #25 on: September 23, 2011, 05:25:25 PM »
 Hmmmm? ok, sorry its really late and I'm really tired, but for you matey,I'll give it a shot ;D  Isnt this what one would call I suppose, a Friedel-Crafts acylation of aromatic systems.. (alkaloids? I reckon there pretty aromatic for some!!!) 8)

 Matey I've had a HUGE day, and a catastrophic fortnight with 6 days of no sleep last week, so I'm going to be brief, however, if there IS something of worth in this path, you can bet your arse, sure ass shit, it WILL BE SHARED..for this MAY BE something new...

 There is already SO MUCH from my pov, data available here ALREADY..that I have as yet have Not Had any dreams to "offer" that had not already been covered elsewhere IF one cares to look..please I mean no insult here for after all, this IS only a Dream yeah?

Anyhow, fuck, i've woken up a bit now and I'm late to go to bed..anyway...

 OK the F-Crafts make carbonyl compounds from aforementioned "aromatic systems", which can then be converted to a corresponding oxime, via..tada! Hydroxlyamine Hcl-
e.g acetylation of benzene to formphenylethanone,to MPK yeah?

Same shovel, different shit

It became known that hydroxlamie Hcl selectively acylates morphine (in its morphenate form) apparently,, at the 6 position exclusively, and to be honest the dream aint over so its hard to say much!!!
The promise Is that,when the dream is a bit clearer, the interesting bits will be told. ALL the Goods Dreamt of Will Be shared...in time, you would not believe how "time" runs in this dream,and its severely 'ghetto' in its work up to a climax, hopefully it will!!!

its just that some "earlier" dreams of this nature, which There Were some Dreams shared, but only a few members noticed, so I had a bit of a limited audience, in the early days,and not that many members were interested in playing around with the things that go on in this dream..and especially now, coz four out of five are no longer here!!!???

   I have a "feeling" I am to be 'on my best behavour' so  finally sharing a few things from a dream can be tricky ..but I'll try to be "Gooder"

I hope that gives you enough of an idea, in fact I dreamt of a steel man sharing love and ideas, which turned out to work well, just, as with most things, it needed a bit of 'modification' which has taken plus grande temps to go by,in this dream, possibly due to MSDS effects :o ;D 8)

 An idea to post a "Complete story" was behind this, and I dont want to disappoint anyone with a shitty ending :'( so as soon as it becomes clearer,you know how Dreams go,ALL will be revealed as apparently tis "poor forum netiquette" I have been accused of, so I'm trying to raise my standard.
   But like I said, I've come across only 4 or 5,  what I think, 'are' novel ideas which have not ALREADY been much thought of/or talked about, SOMEWHERE ELSE, except via a few members, who no longer seem to be around,,or,,whatever.....a Classic example of a "Novel=new Idea method workup whatever,, was jon Now Classic,at least IMHO, route to PA 8) 8) 8) amongst others ??? I hate to say it but Shakey was onto something with his DMA idea....

  A bit like I an NOT SURPRISED AT ALL,  that CERN has virtually PROVEN that some sub atomic particles,neutrinos to be specific, travel faster than light over a 722km distance...which, ahem, poses some slight concerns for many a Physicist, to say the Least! :o Man o steel tis an hour later, you bugger! ;) Its closer to morning than nite so I may just stay up and read a bit, punch a few billies and chill 8)
 
 Anyways G'night all,

peace,love and happy Dreams ;)

 hyppy  8)
« Last Edit: September 23, 2011, 05:28:44 PM by hypnos »
"the two things you can give away and never lose, are what you know, and how you feel...."

reDEEMed

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Re: Re; Hydroxylamine
« Reply #26 on: September 24, 2011, 12:21:55 AM »
I'll let you work you that out then you let me know how it goes lol
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
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hypnos

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Re: Re; Hydroxylamine
« Reply #27 on: September 24, 2011, 12:42:05 AM »
You bet ;)...Its still not quite finished, and currently there's Heaps of M available but  no Hydroxyamine Hcl  at the moment,  waiting on surgery now so eeek, shit! Not good, :o :'( I'm laid up most of the time currently, just Waiting for commands from those Great Gods Known as doctors!!) :o :'(
   I'd say a good 3-4 weeks of dreaming needed here, at least, but thats ok...some mods need to be done in the pre  dream facilitation of required feedstock
  Its being looked forward to, and proceeding,albeit slowly, right now!! 8)

Cheers from Hyppy 8)
who's looking forward to sharing some Quality Love ;D 8)
"the two things you can give away and never lose, are what you know, and how you feel...."

reDEEMed

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Re: Re; Hydroxylamine
« Reply #28 on: September 24, 2011, 12:52:54 AM »
Make the hydroxylamine. It's not difficult at all. I can make hydroxylamine no problem, I cannot get morphine so easily. The reaction you're talking about is just over my head at the moment. I can throw all that shit together and hope for the best but if anything went wrong I wouldn't have any idea what to do about it. I can't quite understand the mechanism, so for now I'll just watch and see how it goes with you. I hope it goes well. I would love to do this reaction, but lack the confidence to risk my materials on it at the moment.

Edit: I'm gonna throw this out there just because I always thought it was interesting and it seems to suit especially what you are talking about doing. I'd sure like to hear how this goes.

Simple Synthesis of Oximes
Summary. The conversion of alicyclic and aliphatic carbonyl compounds as well as aromatic alde-
hydes into the corresponding oximes (up to quantitative yields) was achieved by simply grinding these
reactants, hydroxylamine hydrochloride and sodium hydroxide without solvent. However, this proce-
dure was unsuccessful in the case of aromatic ketones. In this case it was necessary to add silica gel as
a catalyst.
« Last Edit: September 24, 2011, 01:59:10 AM by reDEEMed »
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

hypnos

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Re: Re; Hydroxylamine
« Reply #29 on: September 25, 2011, 03:55:08 AM »
Man o man, I just Lost a HUGE THANK YOU post to you reDEEMed along with a whole lot of other stuff I just lost into cyber space!!! :'(

 Shit!  >:(

Anyway thanx A LOT for that reference, 8) 8) 8) yeah, the PTC ideas been floating around a while, BUT
the "grinding of DRY hydroxylamine Hcl" even after All the  comments on this post, feels a bit like a "You Go First!" activity  :o  Doesnt sit well with me, just yet,
    And it Is a Serbian paper, and with many such friends, its known they can be Mad bastards-NO OFFENCE Intended,, just like a dear Israeli Grrrrlfriend,who like most of them, "Is Interesting in her approach!!!" to say the least!

 But THANX AGAIN, Man O S once Again, you totally "accidentally" find the Good OIL, Nice One ;D 8)...I'll keep you posted

Cheers all, and what do we think of Grinding  "dry Hdroxylamine Hcl in a Mortar and pestle?" ???

Hyppy  8)
"the two things you can give away and never lose, are what you know, and how you feel...."

reDEEMed

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Re: Re; Hydroxylamine
« Reply #30 on: September 25, 2011, 05:32:28 AM »
I would do it. The salt is stable as can be. There are no worries of explosion when dealing with a salt of.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

hypnos

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Re: Re; Hydroxylamine
« Reply #31 on: September 26, 2011, 04:44:32 AM »
 Steely, considering all the input from other members, it seems it "should be" OK...that said...and considering lugh's comments,  I wonder HOW it is POSSIBLE, for trained Commercial chemists, in Professionally run (one Would Imagine...) Facilities,, Manufacturing, this, and most likely, other chemicals,,to end up with an Industrial Scale Fuck Up, which " BLOWS UP, YOUR FACTORY???!!!" :o :o :o

  Far Out!!!  Talk about "Lab Accidents, and Runaway rxn's!!!"  :o  ;D  ???

   My Francaise is weak, at best, Yet I have some doubts, lugh would post "irrelevant references",, :-\
     
 Ergo;...hey lugh, I humbly ask if you, or Anyone else,, who DOES KNOW how, or "the cause" as to WHY?,, these factories, as recently as 1999, came to Explode, whilst manufacturing this compound???

   I've looked, but had little success with details re: these Industrial Explosions, other than a few Newspaper ugh..'articles' hyping with the "Scare Value" of these incidents!!
   
  (RR, if you Could be Bothered I could do with some translation help  :P :), however, that could mean, translating several papers, :P for what may, or may Not be, 1, a 'fair and reasonable' thing to ask of you, however, you Did offer.. ;D 8)..!',,,
    and 2, after ALL that, there, May, or May Not, be data which I would find useful--I would more than likely,...
   I think, that "YES, there IS a High Possibility, they hold data, of which I know Not!) however I wouldnt 'Know'this,, "UNTIL I HAD read them" ???....hmmmm...bit of a Catch-22 here, if you know what I mean!..If not, just ask  8) 8)

   Looking forward to some More Cool pov's, Facts and Referrals AND Translations--sometimes "translation programs",, I have used before,( particularly upon, those languages, Like French, Italian,German etc, with, "arse about, sentence structures",) do not "translate well" ??? :o :P....
           ESPECIALLY scientific papers,, And, can be for me, like Ikea instructions, with a page missing!!! :-\ :P ::)...I just "dont quite get what they are saying, YET, because, I KNOW, "what they are getting at" and can sometime "join the dots" quite successfully!!! Far from always, though!

  BTW.. Rdmd, dont you worry about "unsuccessful" attempts ???...I kind of Expect, at Least several,..thats Not being, pessimistic, just realistic ( oh well )...
   When one is trying, with High quality, Ghetto Equipment ( howz that for an Oxymoron!) I am stumbling along sloowly. 8)

   I dont consider, 'unsuccessful experiments' as Failures, they ARE PART OF the learning curve!!! :o ??? 8) Matey,,,WHO HAS,,M to "fuck around with" NOT ME!!!

 my dreams are Very small scale, in many respects,,but I dont Limit "their Possibilities!",,as they say "Argue for your limitations, and they SURELY Will Be,,Yours"

   However, It's available, for "careful Experimentation, on a Small Scale, and It DONT come Cheaply
 
 Cheers amigos, thanx for the input ;D

   Now WHO has Tried GRINDING,, Any form of Hydroxylamine compounds salts OR otherwise? :o 

  I havent....and Would like to KNOW more ???

  Hyppy 8)
« Last Edit: September 26, 2011, 04:48:43 AM by hypnos »
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Tsathoggua

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Re: Re; Hydroxylamine
« Reply #32 on: September 26, 2011, 06:24:09 AM »
Distilling the freebase, at least in some cases I have read of has made the odd factory go kablooey, particularly in the presence of NaOH (and presumably other strong bases)
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reDEEMed

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Re: Re; Hydroxylamine
« Reply #33 on: September 28, 2011, 08:46:16 PM »
I just found solid fucking gold.

The chemistry of hydroxylamines, oximes and hydroxamic acids

You can download it in the references section. I highly suggest this book to get inside hydroxylamine's head as well as having a proper treatise into the mechanism of oximation, which I found lacking in every other major textbook, even the venerable March's.

http://127.0.0.1/talk/index.php/topic,794.msg26305.html#msg26305

Edit: hehe have a look at compound 120 in the book. I swear I've saw that somewhere before.
« Last Edit: September 29, 2011, 02:12:56 AM by reDEEMed »
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

reDEEMed

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Re: Re; Hydroxylamine
« Reply #34 on: September 30, 2011, 11:11:27 PM »
I decided I wanted to see if I could make Hydroxylamine sulfate the way ShroomedAlice did. One thing I do love about chemistry is one of the same things I used to love in the machine shop, improvisation. This setup today has got to take the cake as far as stretching the intended use of this glassware. I love the challenge, though, and I think I succeeded, we'll see. I really want to find a reliably high yielding synth for this shit because I wanna oximate ever fucking thing lol. I really can't explain the fascination, maybe it'll go away after I do a few compounds, but right now the shit is full force. In addition to wanting to make formaldoxime, it occurred to me that acetone can also be fucked with by this magical dust. I have a little reading to do, to make sure I don't make something nasty that might endanger me or my girl, but I really hope to start some sort of oxime experimentation tonight, probably with acetone.

Some pics of my setup. The more Rube Goldberg it gets, the happier I am ;D


Edit: My addition funnel is a 50ml buret that I need a ladder to get to the top of so I can top it off when it runs low. Also you can see all the odd pieces I stuck on to attach a vent line to vent the carbon monoxide outside with.
« Last Edit: September 30, 2011, 11:15:45 PM by reDEEMed »
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

RoidRage

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Re: Re; Hydroxylamine
« Reply #35 on: October 01, 2011, 12:06:16 AM »
Nice setup ;D Keep up updated, I'm really interested in that reaction. I have the original german patent around somewhere than I need to translate one day but I won't if it works as advertised ;D.

reDEEMed

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Re: Re; Hydroxylamine
« Reply #36 on: October 01, 2011, 05:58:50 AM »
Well, as usual I fucked it up from the beginning, so I'll have to try again. I pretty much count on that anytime I do anything. I'm not sure if that's a good attitude to have or not, but that's how it is lol. I really rushed into this and didn't really prepare, mainly I didn't read the patents thoroughly. But also I had some other shit going on when I started this, household type thangs, and I was distracted by said thangs. Rather than drip the shit in over a couple hours I dripped it in over closer to five hours. It wasn't till just a little while ago that I finally reread the post by Alice and realised how far off I was. My timeline looked more like- Heat to 80 then start dripping in H2SO4 at about a drop or two every 3-4 seconds, stirring pretty hard the whole time. About an hour in, start dripping about a drop a second and increase heat to get a good steady reflux. Since I didn't even bother to glance at a clock, I can't say exactly how long I did this, about 5+ hours.

Some other shit came up and I could not do the reading I had planned. I wasn't sure about the whole mix with alcohol and let cool thing. I quickly scrolled through the relevant patents and that other paper that was attached here, but couldn't really find what he meant by alcohol, so I used methanol. I just doubled the weight of the reaction solution with methanol, then put that mixture in a sealed mason jar outside to cool.

But that's not all, I'm good for atleast three fuck ups. I was looking at the equation for the reaction. basically looking to see how the CO came into play. That's when I saw the +H2O on the left side over there. I didn't add any water.

So, I'm not sure how big a failure or success it was yet. As of right now I have nothing solid, maybe that will change, I dunno. I will be doing it again either way, just with more preparation next time.

"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

reDEEMed

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Re: Re; Hydroxylamine
« Reply #37 on: October 01, 2011, 06:02:38 PM »
I can't tell whether Alice dripped in his H2SO4 and then refluxed for three more hours or if he refluxed for three hours then dripped in his acid. Where ever he picked this procedure up it's buried in one of these refs I suppose. It certainly is not the main procedure that is outlined in any of them. I would like to know which one he used as a guide for putting his procedure together.

Even after all night I have nothing at all. I will try the oxylic acid route today if I can ever motivate. I kinda wanna try this way again, though.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

reDEEMed

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Re: Re; Hydroxylamine
« Reply #38 on: October 02, 2011, 09:49:04 PM »
I'm having trouble finding whatever ref it is Alice used to build his procedure and just his post is not enough to replicate the results. Upon putting solution in the freezer until atleast 0c throughout, still nothing. I took the jar out of the fridge and allowed it to come up to room temperature. I then tried to oen the jar, but the now reduced pressure in the jar made that difficult. With some effort the lid finally lifted up giving a loud pop as the air rushed in. I swirled around a minute looking at it and sniffing it. It should smell of acetic acid at the very least, and it did. I still have no idea why I did it, but I put the lid back on and put it back in the freezer. Some time later I decided that I would try to distill everything back out and try again. When I went to get the jar I was totally shocked to see a layer of crystals on the bottom about 6mm thick and patches of crystals here and there. The crystals were star shaped, about 3-4mm in diameter and very clear. I filtered these off and back in the freezer the jar went. Once it will no longer give up crystals I will distill down, refreeze, distill, refreeze etc until I get through it all.

I put in a request for the article I believe to be the one a guy named Preibisch published in the late 1800's detailing his findings that a primary nitroparaffin heated with a mineral acid will give the corresponding acid salt of hydroxylamine and some other stuff. If I can get this paper or any paper that details the procedure Alice did, maybe I could replicate the results, but I don't have enough right now to do it.

RoidRage, you say you got a german patent for this? Can I/we see it?

Here's the first crop of what I assume to hydroxylamine sulfate. If nothing else they are very pretty.
 
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

RoidRage

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Re: Re; Hydroxylamine
« Reply #39 on: October 02, 2011, 11:18:29 PM »
Wow really nice work there reDEEMed. Those crystals are definitly beautiful :).


As for the original german reference, here it is. I wasn't able to directly upload it on the site (Dunno why though, it's not over the max size limit) so I uploaded it here: http://ifile.it/3pgbdko ... It's the whole volume, which is 481 pages. What you need to look at is page 480. It's Preibish's work titled ''Uber Nitrocarbol''
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