Author Topic: Hydrazine, and substitutable amines.  (Read 4252 times)

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madchemist

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Hydrazine, and substitutable amines.
« on: September 29, 2000, 02:51:00 PM »
In the LSD synthesis I was looking at, it said diethylamine can be replaced by many similar amines.  One of them is dimethylamine.  Could this be made from some methylamine HCl?  How would one go about adding an extra methyl group?

  Also where can I find hydrazine?  Is it watched?  Can it be produced from non-watched precursors in the home lab conditions?  I have a good understanding of chemical procedures, so throw them at me.  I have done many searches on this to no avail.

MTM

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Re: Hydrazine, and substitutable amines.
« Reply #1 on: September 29, 2000, 05:26:00 PM »
Don´t want to flame you, but you ask in the newbee forum how to synt. HCl and now you´re talking about LSD synth.
Hint: Forget it!


---MTM´s still waiting---

halfapint

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Re: Hydrazine, and substitutable amines.
« Reply #2 on: September 29, 2000, 07:06:00 PM »
DIAMIDE, OR HYDRAZINE, NH2-NH2
    This compound of two unsaturated amidogen (NH4) groups or radicles is prepared by interaction between sodium hypochlorite and ammonia whereby chloramine is produced: NH3 + NaOCl = NH2Cl + NaOH. If this be distilled at a low temperature in an atmosphere of ammonia, in vacuo, hydrazine hydrochloride forms, NH2Cl + NH3 = NH2.NH2.HCl.
    Free hydrazine is obtained by distilling its hydrate or sulphate in a current of hydrogen under reduced pressure with barium oxide:

             N2H4.H2O + BaO = Ba(OH)2 + N2H4

Hydrazine is a colorless liquid which boils at 113.5o, solidifies at 0o, and dissolves in water with formation of a hydrate, N2H4.2H2O. After evaporation of the water N2H4.H2O remains. Hydrazine is exceedingly alkaline and with acids forms two classes of salts, N2H4.HCl and N2H4.2HCl. It is not explosive and is readily distinguished from ammonia by its reducing power.



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that I erroneously attributed to a 1916 book in another thread. With a bit of study, I was hoping a synth could bee worked out from what's said here. Let's see, it would have mw about 32, that's light. From what I think I've seen on its toxicity, or imagine I have, I'd sooner not trust my nose on this one; probably a very labile liquid, with what I'd expect to be a high vapor pressure. They show a derivation from the hydrochloride, then show how to get free base from the hydrate or sulfate, so there's a gap there. Presumably you could get the hydrate by neutralizing with equivalent sodium ions, like the hydroxide, and concentrating from water. Would I expect the salt to drop out? Wouldn't bee surprised to see it precipitate.

So this stuff ought to be kept under cover, pretty much inside glass. A current of hydrogen over barium oxide, barytra? No, think that's a mineral name. These sharply reducing and dehydrating conditions sound about right for the "diamide" so closely related to ammonia, only doubly so. Wonder if this shit detonates under some exciting circumstance. Most simple nitrogen compounds tend to do that. Let's keep the shit real tranquil until we find out, that means chill, that means use the vacuum. Wonder if somebody's gonna contrib a synth, better bee a real trustworthy one. Better bee at least as good as mixing chlorox and aqua ammonia.


turning science fact into << science fiction >>

halfapint

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Re: Hydrazine, and substitutable amines.
« Reply #3 on: September 29, 2000, 08:27:00 PM »
Yeah, I see it's not explosive, by my own citation. Actually didn't cite. Pharmceutical and Medicinal Chemistry, 1918. Incomplete but there. arrgh, didn't want to post again, have to figure out the mw of NaOCl and do moles. Hate moles, they're so quantitative. OK, 23 + 16 + uh, 35.46 = 74.5. Hydrazine I said's 32? Ammonia would bee 17. 4.38, say the molar ratio's 4.4 times as much NaOCl needs to react as ammonia. Household bleach is standardized Javelle water, 5.25%. Ammonia is 28% or 30% lab grade, 3% household. Household ammonia's cheaper, white not sudsing nor scented nor any other additive.

So we want to come out with a volumetric answer here, for convenience. Say the percentages are w/v. Is that right? hmm. Sodium hypochlorite is 0.0525 of the composition of bleach, the other 94.75% being water. Nominally we disregard the other chlorine species actually present, temperature dependent, etc., in bleach, expecting them to show up in yield loss. Remembering constantly that oxidized chlorine species also tend to explode on excitation, but such species are largely supressed in the presence of sodium ions, or for that matter by ammonium ions. Whew, squeaked by on that one too, without introducing any possibility of a blowup. The vacuum is needed for yield anyway.

Where were we? Ammonia is 0.03 of the composition of ammonia water. Hate arithmetic, it's got too many numbers. Am I blasted? Maybee a better idea to come back to this.


turning science fact into << science fiction >>

madchemist

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Re: Hydrazine, and substitutable amines.
« Reply #4 on: September 29, 2000, 11:39:00 PM »
I said in the other posts I want to try to synthesize HCl acid becuase it helps save money (around here it is hard to find and expensive),and the less chemicals you buy the less suspicious.  I am not stupid.  In my opinion LSD production is not a hard thing to do.  I wonder why everybody are such assholes on this site.

terbium

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Re: Hydrazine, and substitutable amines.
« Reply #5 on: September 30, 2000, 02:54:00 AM »

  I said in the other posts I want to try to synthesize HCl acid becuase it helps save money (around here it is hard to find and expensive)


They don't have swimming pools where you live?


Drug_Phreak

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Re: Hydrazine, and substitutable amines.
« Reply #6 on: October 01, 2000, 05:05:00 AM »
Madchemist, you should buy Practical LSD Manufacture by Fester. He explains how to make anhydrous hydrazine from very mundane OTC chemicals. Instead of substituting amines... is there any chemical that could be used as a substitute for anhydrous hydrazine?


____________________________

Society exists by chemical affinity, and not otherwise.

terbium

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Instead of hydrazine.
« Reply #7 on: October 01, 2000, 07:30:00 AM »
Shulgin in TIHKAL lists a number of methods for for coupling the amine with the lysergic acid. Using hydrazine is not one of them. I guess that with the hydrazine method you must reflux lysergic acid with anhydrous hydrazine to produce a hydrazide and then displace the hydrazide hydrazine with the amine. Shulgin likes using POCl3 as the coupling agent. Other coupling agents that have been used for producing LSD are carbodiimides and SO3, both mentioned in TIHKAL.

terbium

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Lysergic acid dimethylamide - DAM-57
« Reply #8 on: October 01, 2000, 07:36:00 AM »
According to TIHKAL the dimethhylamide does not seem very promising: "This compund did induce autonomic disturbances at oral levels some ten times the dosgae required for LSD, presumably in the high hundreds of micrograms. There is some disagreement as to whether there were psychic changes observed."

Drug_Phreak

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Re: Lysergic acid dimethylamide - DAM-57
« Reply #9 on: October 01, 2000, 01:07:00 PM »
Actually the good thing about the anhydrous hydrazine method is that someone can start from LSA instead of having to use lysergic acid as a starting material, so let me re-phrase my question (I should of been more clear to begin with)... does anyone know of a chemical that could be substituted for anhydrous hydrazine in Fester's one pot shot method (which is in his LSD book) that would still give superior results like the anhydrous hydrazine procedure does? 


____________________________

Society exists by chemical affinity, and not otherwise.

madchemist

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Re: Lysergic acid dimethylamide - DAM-57
« Reply #10 on: October 01, 2000, 08:49:00 PM »
I'm not worried about the hydrazine any more.  The method described above is valid, because I saw the same things on Rhodium.
  The diethylamine is what I'm worried about.  But I also read some where it can be procured from making ethylamine.
Here is the link:

http://rhodium.lycaeum.org/chemistry/tcboe/chapter9.html


Drug_Phreak

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Re: Lysergic acid dimethylamide - DAM-57
« Reply #11 on: October 02, 2000, 11:09:00 AM »
I guess there isn't one huh? I don't think anything could come close to hoffman's synthesis anyway. Fester has a decent procedure for making diethylamine in his book. Also, the synthesis of diethylamine will produce similar amines as by-products... just like synthesizing the other popular amines. There's no reason to get it by making ethylamine when you can just make diethylamine itself. If I remember correctly... to get a high yield of the desired amine, one has to keep a close eye on the temp, and reaction time etc... unless they'll end up with a blend of amines in different percentages that will need a lot of fractional distilling. You have been warned... arr fukin muhahahaa.


____________________________

Society exists by chemical affinity, and not otherwise.

Osmium

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Re: Lysergic acid dimethylamide - DAM-57
« Reply #12 on: October 02, 2000, 11:46:00 AM »
OH MY GOD!  ::)

Newbees shouldn't work with hydrazine. Period. And LSD production isn't for newbees either. Just forget it, k?

Since it's monday and I'm usually generous on mondays here's a synth for hydrazine sulfate:

In a 750ml erlenmeyer flask 165ml conc. NH3, 35ml water and some animal glue solution are mixed. (The animal glue solution consists of animal proteins and will remove traces of heavy metals, gelatin might substitute here, or simply use reagent grade chems to start with). NaOCl solution is prepared by bubbling Cl2 into 100ml 2N NaOH solution until the weight has increased by 6g. This is less than the stoichometric amount, because presence of free Cl2 has to be avoided. This NaOCl solution is poured into the ammonia and heated to boiling. Evaporate about half of the water. Then cool with water, next with ice. Add conc. H2SO4 dropwise to precipitate the sulfate. Recrystallize from the least amount of water possible.

Don't try this at home, hydrazine is some nasty shit.

madchemist

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Re: Lysergic acid dimethylamide - DAM-57
« Reply #13 on: October 02, 2000, 11:34:00 PM »
I am probably going to put off on the acid for a while.  I am not to much of a newbee, since I've made several of small batches of X and meth through the lueckart reaction (some a success, some not, but i am now leaning more toward constant success).  I am going to get a few more of these under my belt, as well as try a couple of new things.  Thanks anyway!