Newsgroups: alt.drugs.chemistry
From: [an 216208] at [anon.penet.fi]
Date: Thu,  2 Nov 1995 10:34:22 UTC
Subject: *ZWITTERION* - on making Cyanogen Bromide


I WOULD apologize for the length of this post, but if you want to make
Cyanogen Bromide, then you BETTER FUCKING READ THIS! I've committed all the
GOOD FUCK-UPS for you, so LEARN from my MISTAKES!

Ha.ha.ha.ha. Boy that Eleusis is such a funny guy. Yes, he's served up quite
a TASTY LITTLE SMORGASBORD OF CYTOCHROME OXIDASE INHIBITORS with this one.

GOD I AM FUCKING LUCKY TO BE ALIVE, MUCH LESS HAVE THE MOTOR SKILLS TO TYPE
THIS FRIGGIN' POST!!!!

Having experienced the SENSUOUS delight of nearly burning my "lab" down
making isosafrole, I then felt it my HUMBLE duty to attempt making Cyanogen
Bromide.

I mean, HEY, I'm here to test out WHATEVER get's posted to this group in the
way of SYNTHESES, and since e-freakin'-leusis is the only TARGET to pick on,
I suppose I have to live with whatever he SPEWS upon this group.

So, here is what ZWITTERION did in making cyanogen bromide, SO FAR, because
ZWITTERION is NOT DONE YET:

I dunked a RB flask into a water bath with a couple of pathetic cubes of
ice. I measured out 50g of AR Bromine and added this. Fumes, fumes,
everywhere I tell ya. I quickly added 5mL of water and plugged the flask
with a ground glass stopper.

While the flask was chillin', I measured out 17g of AR Sodium Cyanide,
anhydrous, and dissolved into 120mL of room temp. water. It required a bit
of gentle stirring, but went completely into solution within 3 minutes. A
couple of grains got on my bench top to which I said "Say, that stuff's
deliquescent, ain't it?". I promised to clean it up with an HCl dampened
sponge later, but for now, my delicate and loving pressure equalized
addition funnel was calling for me to load it.

I quickly replaced the stopper with the addition funnel, then stoppered the
funnel. Bromine fumes crept noiselessly up the return arm and suffused the
entire setup. It was quite a lovely sight, really. I loaded the funnel,
started the magnetic stirrer, and let the solution drip at about 1 drop
every 2 seconds into the flask.

After about 80mL of cyanide solution dropped into the flask, I noticed lots
of needle shaped colourless crystals all about. The reaction mixture was
starting to get a little chunky with crystals as well. With the last 40mL,
the Bromine vapor disappeared as it became consumed with envy for the
cyanide ion and the reaction mixture turned blackish-red. Crystals were all
over the flask now but I let it react about 15 minutes past the
disappearance of the Bromine.

Total reaction time: 2 hours, 30 minutes. Not bad, E.

Oh, did I mention that I don't have a fume hood? Hahaha, yep. I threw
caution to the wind on this one. Oh ya, my lab is really my apartment, so
this is INDOORS, even.

Now it was time to DISTILL! Ahhhhh, what fun!

So I removed the addition funnel from the flask and, oops, here comes some
noxious fumes right in my face! My eyes were searing, I thought I smelled
almonds, but I wasn't sure because the stench of Bromine was too strong. Bad
move, so I capped the flask and took a smoke break. Ummmm. I love the smell
of Bromine in the Evening! Or, at least I THOUGHT it was Bromine. No such
luck, that was the smell of Cyanogen Bromide! Yes! I've been breathing this
shit in like it was Christmas Come Early! For the love of God, Give me MORE!

Try #2: I assembled an RB flask to a 3-way adapter and a vacuum receiver
adapter, but when I tried to distill off the BrCN, it clogged up the
receiver adapter, releasing more toxic, acrid fumes into the room. You know,
I REALLY ought to rig up some sort of fume hood - E's not kidding about this
SHIT! 

TRY #3: So, I took it apart AGAIN, and plugged the receiver flask directly
into the sidearm of the 3-way. Too bad I left my goggles hanging on my car's
REARVIEW MIRROR. Ahh.. Who needs eyeballs anyway. Damn I'm getting tired of
that smell... or is that smell making me tired? I finally just picked the
whole damn lattice up and took it out to my patio - OUTSIDE WHERE IT SHOULD
HAVE BEEN IN THE FIRST FUCKING PLACE. There, much better.

I preheated a pot of water to boiling, then slid that underneath the
reaction flask. Distillation commenced smoothly right at about 60C on my
thermometer. I had to wrap the 3-way adapter and receiver flask neck with
aluminum foil to prevent clogging, but within an hour, the temp. fell,
indicating NO MORE BrCN vapor. The whole inside of the RB flask was covered
with a layer of whitish-clear needle shaped crystals. A quick perusal of the
Merck says this is just what it should look like. Fantastic!

ZWITTERION then disassembles the setup, plugs the receiver flask, and plops
it in the FREEZER for tomorrow. I am doing this to see if it will BLOW UP
overnight. Either way, in the next post I will give the YIELD or the NUMBER
OF GLASS SHARDS.

All in All, a nice bit of entertainment. The smell of Cyanogen Bromide
reminds me distinctly of the Isocyanates, the unstable intermediates when
making METHYLAMINE via Hofmann degradation. It's nice to note that an
Isocyanate is what KILLED ALL THOSE POOR LITTLE INDIANS IN BHOPAL!

So, grudgingly I accept Eleusis's TRANSCRIPTION as basically valid. I TRIED
TO SCREW UP EVERYTHING I COULD, and, well, I screwed up. My suggestions to E
for improvements to his document ARE HERE, so COME AND GET 'EM, E-BOY.

Maybe POPeye will post something SAFE for me to try.. A NICE BIRCH REDUCTION
would go well at this point...

END TRANSMISSION
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