Author Topic: Question on reductions using LAH  (Read 1812 times)

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LeVogue

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Question on reductions using LAH
« on: March 05, 2001, 05:29:00 AM »
I've noticed many individuals who chooses alternative methods for reductions of nitropropenes/styrenes rather than Shulgins favorite (high-yielding) method with LAH.

I know it can be a problem to obtain LAH, but a guy i saw on TV bought some, and now he's thinking about just forgetting the whole thing and pick another method to reduce his P2NP to Amphetamine.

Is it really that hard/dangerous to work with, or would there be a chance that the guy could move on without any fear and reflux his nitropropene with it ?

Maybe someone who knows the chemical could explain a few things about reductions with LAH. Personally i'm sure that the guy from TV could use some information on where the common mistakes are made.


-Le Vogue

Rhodium

  • Guest
Re: Question on reductions using LAH
« Reply #1 on: March 05, 2001, 06:31:00 AM »
This contains some valuable advice:

http://rhodium.lycaeum.org/chemistry/eleusis/zwit.2c-h.html



Main points: Use Sodium-dried solvents, add the nitrostyrene solution SLOWLY, and make sure you use a dust mask so you dont inhale any of the very fine LAH dust, which easily disperses into the air.



http://rhodium.lycaeum.org


foxy2

  • Guest
Re: Question on reductions using LAH
« Reply #2 on: March 05, 2001, 06:47:00 AM »
Why not save the LAH for something more interesting?
You could reduce the P2NP with one of the lower yeilding methods.
Shit you could reduce phenylalanine with the LAH to amphetamine and you would end up with more.


Do Your Part To Win The War

yellium

  • Guest
Re: Question on reductions using LAH
« Reply #3 on: March 05, 2001, 12:03:00 PM »
Sodium drying of THF (with benzophenone as indicator) is not recommended for quick&dirty work. Takes way to long, and when the Na has done its job after 2 days then you need to distill your THF.  Of course, if you work in a real lab, you can make a dedicated THF drying setup, just like the pros.

For me, drying your (not-to-wet) THF or ether with CaSO4, and then adding slightly more LAH also does the job. Another quick&dirty way is adding NaH (if you can get that) to your THF until it doesn't fiz anymore. Let it stand for a while, decant of the amount of THF you want to use onto your LAH...presto!

Dust mask? Nah. Gloves.

OTOH: LAH for amph? I would save it for 2C-B. Unless you don't like visual drugs.

Yellium `I love the smell of bromine in the evening'

terbium

  • Guest
Re: Question on reductions using LAH
« Reply #4 on: March 05, 2001, 10:08:00 PM »
Re

Post 63698 (missing)

(LeVogue: "LAH to acetic acid ester of eph", Newbee Forum)
. The guy on TV should take his LAH out of the fridge and let warm to room temp. before opening the can. Don't want any moisture condensing on the LAH.

LeVogue

  • Guest
Re: Question on reductions using LAH
« Reply #5 on: March 09, 2001, 06:03:00 AM »
The LAH the TV guy was talking about was in tablet form and was only to be stored in cold dry places, of couse sealed in the way the Chem supply house had. Now he's to busy posting, so i'm doing the job or him, hehe .. ehm ..(those tv chemists work like hell).

OK, back to the main question.
It was what needed was, just some info on it so explosions hopefully didn't happen.

foxy :


Shit you could reduce phenylalanine with the LAH to amphetamine and you would end up with more.


I've never seen postings about reduction of phenylanaline with LAH to Amphetamine.
Curious, if anyone you/someone had something about it lying around.

Yea, 2C-B is cool, but the synthesis is a bit of time consuming process, and bromine is not the nicest chemical to play with.

Thanks for the help  :)


-Le Vogue


yellium

  • Guest
Re: Question on reductions using LAH
« Reply #6 on: March 09, 2001, 09:21:00 AM »
LAH in tablet form sucks. Powder is way better.


>2C-B is cool, but the synthesis is a bit of time consuming process

WTF? The first step (formation of the styrene) takes two days of unattended reaction if you follow rhodium's henry reaction (with ethylenediamine tetraacetate). The reduction takes just as long as the amph reduction would. OK, brominating after work-up. That'll cost you an evening. But you'll end up with a lifetime stock of a compound that's *not* neurotoxic.

But the difficult part is getting the aldehyde. OTOH, if you can get LAH...

And indeed, you should wear gloves when handling bromine. But you needed these gloves anyway for LAH.

LeVogue

  • Guest
Re: Question on reductions using LAH
« Reply #7 on: March 13, 2001, 10:31:00 AM »
I don't know which form of LAH is the best, cause i've never used that chemical before. (And i'm getting a LAH-fobia soon, i just keep finding Warnings and Road hazards about that unstable stuff). I only bought it as a substitute for NaBH4, cause borohydride is toxic labeled and unable to purchase.

How about this reducing agent :
Sodium Aluminum Hydride Bis-(Methoxyethoxide) - aka. ' Red/Al ' ?

Is it really better than LAH ?
If so, i wonder why it only appears in one synthesis at Rhodiums page.

-Le Vogue

yellium

  • Guest
Re: Question on reductions using LAH
« Reply #8 on: March 13, 2001, 12:53:00 PM »
Red-Al might be less dangerous than LAH, but that's mainly because you
don't have to sit next to a setup with THF at reflux temp. If you're doing
these reactions at your home, without a proper fumehood etc, but with lots
of ignition sources, I would be more scared of THF than of LAH.
I wouldn't want to cover my house with THF or ether fumes.
When you quench the reaction, you have to be just as careful when adding
isopropanol or water.


For a `typical' reaction employing Red-Al, see

http://www.erowid.org/library/books_online/tihkal/tihkal33.shtml


Note: the water wash is important. You don't want to eat methoxyethanol.

The reason that it only appears in one synth is that it is a more `professional' chemical. Ever wondered why you don't see that much synths employing borane or buli on rhodiums page? Same thing.

LeVogue

  • Guest
Re: Question on reductions using LAH
« Reply #9 on: April 06, 2001, 11:47:00 AM »
Hi there ...

I got a visit from the Narco Swines, and i've just got released from jail, and i can look forward to more time in there.

Not that my post has anything about the topic to do, but i just wanted to give a greeting to my fellow bees.

I lost for about $2500 labgear, and it sucks.
Much of my chemicals such as 500mL Nitroethane was unbroken bottles, and that sucks too.
My Benzaldehyde, my metalhydrides and this and that of goodies !!

I'm like needing to have a break, and just want to greet you all, and ok i fire this this cliché off too : Be aware of the swines, they tap your phone(s), they follow you everywhere, and snap photos !!

Take care everybody, thanks for the help in the past !!

-Le Vogue 


What comes up, comes down, comes up, ..... YEP! ..... and down again !

terbium

  • Guest
Re: Question on reductions using LAH
« Reply #10 on: April 07, 2001, 09:29:00 PM »
I am very sorry to hear of your misfortune. Any information you feel you could share on how this happened could be instructive to all.

LeVogue

  • Guest
Re: Question on reductions using LAH
« Reply #11 on: April 09, 2001, 03:05:00 AM »
I guess it depends on where you live.

My case was that i got a 'complete' list of the chemicals that suppliers was to inform the 'narco swines' about.

But unfortunately it wasn't a complete list, and something turned out to be shit in my face.

Don't trust anyone, but yourself.

-Le Vogue


What comes up, comes down, comes up, ..... YEP! ..... and down again !