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  Subject we need an updated ketone/nitro writeup   Reply  
  Posted by muriatic_asshole (Hive Bee)  
  Posted on 11-14-00 02:00  
 
methyl man and baal, can you guys put together a summary of what you think is the easiest and best nitro method and also for ketone production.  it's hard to wade through all of the recent posts.  we need a fresh update.  because of its otc'ness this looks like the sweetest and easiest method for aspiring apiary workers.



MM thanks for all your hard work on this.  I've been following your posts for around a year now.

DrHoNow!  call the number on your screen!
3 easy payments!  beautiful carrying case!
  
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by pmpB_4 (Stranger)  
  Posted on 11-14-00 22:20  
 
since you asked soo nicely here you  go!
50g of good mdp2p
1500 ml of meoh or etoh or ipa
55g al
let al and hgcl2 amalgate until grey alcohol and bubbling!
then
add 5 ml nitro to the mix
then add 45g nitro/50g ketone
at 3 drops per second, use 2 400-600mm condensers
if addition is faster and add more alcohol when needed to keep it stirring
add it a;l within 30 minutes
note use at least 3000ml fbf for every 50g ketone
when the mix starts to slow down add heat and reflux at medium reflux temp for 3-4 more additionAL hours. then allow to cool and mix for 3-4 more hours, if you want to evap alot of the meoh
then make basic with koh/naoh solution then extract 3x with no less than 1200ml tol for every 50g
workup as usual.
if the tol is very basic 10+ph the mix is full of the good stuff!
yields of 40+g of product will always follow everytime
if anyone wants to dispute (ab2, placebo other little shittalking bitches)this go ahead, not a chemist here but a fulltime dreamer. this route is followed 4-6x a week at up to 200g. don't play around with small stuff!
if not getting these yields you have either impure ketone, or improper amalgation, or bad lab technique.
hope this helps for anybody that needs help in this route if any q's arise pm me!
pmpB_4
coolcoollaughsmile
only E pimp's like swinpmb_4
make things happen (jk) 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by zooligan (Hive Addict)  
  Posted on 11-15-00 00:08  
 
In reply to:

use 2 400-600mm condensers


Damn!  That's a lotta cooling power.  Does the reaction run that hot with just 50g, or are you talking for something bigger??

z

 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by Antibody2 ()  
  Posted on 11-15-00 03:09  
 
heard that frostsmile 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by hitman (Stranger)  
  Posted on 11-15-00 12:31  
 
Are you guys using Liebig-condensers? tongue

Wouldn't ONE 400mm Graham-condenser be enough to cool this baby? smile
Ooooops I did it again!.... 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by baalchemist (Hive Bee / Eraser)  
  Posted on 11-16-00 23:26  
 
I was planning on putting together a more detailed write-up on this subject with all the quirks dealt with more explicitly.  The higher end yields that Baal accomplishes(50g's+ from 50g-K) require some strict parameters to be followed and the cues to look for when initiating them. In recent posted improvements to this reaction, I had posted reactions details that really didnt stress area's of cruciality that definately make the difference in the higher yield. SWIM is about to start working on a website that will have Baalchemists complete pictorial "OTCXTC" routes along with precursor construction techniques. This will provide a more detailed account on those kinds of particulars of all the different reactions SWIM uses to get those higher end yields. The website will provide the necessary info on how one can produce over 5lbs of snow-white powder from 1 gallon of oil and ~$400 in otc chems & solvents, and a shitload of labtime. Site should be up by 1/1/2001.
 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by Methyl_Man (Hive Bee)  
  Posted on 11-17-00 09:55  
 
The fictional character known as Methyl_Man hereby respectfully hands over the perceived mantle of Al/Hg/nitro monarchy to baalchemist. He is the only one who has put in more time and done this reaction more times than MM, as far as MM can tell. He has advanced the knowledge more than MM at this point. More power to him. In fact though, MM's niche was always more in describing the process in detail than in maximizing yields. baalchemist has gotten even more intimate with the parameters. This is good and will forward the "science" of it even further.

Just to throw in a nod, yes, MUCHO cooling power with this is needed if you want to run it fast and hot and get good yields. At the 55g aluminum scale, one 400mm Allihn isn't enough, and one 300mm Allihn is DEFINITELY not enough. I dream of a super heavy-duty mega cooling setup that would allow one to practically just dump the ketone in all at once and do the reaction all in about a half hour. The energy released by a fast amalgamation at the 50g aluminum (and above, no doubt) scale is amazing.

One key factor---and baal and I are in agreement on this---is that there is a "spike" in the middle of the amalgamation process, a place where it gets hottest based on how fast the ketone had been added up to that point. Assuming a decent rate of addition in the beginning, like around 2 drops per second, with experience one can take the reaction to the brink of volcano-ness---the spike---and then stop the addition for about a minute, let it calm down, and then from that point forward it is less subject to go nuts and one can speed up the addition significantly (with caution of course). Yields are ABSOLUTELY LINKED to the rate the ketone goes in versus the rate of amalgamation. In other words, if the aluminum looks mostly reacted, and you still have half your ketone in the addition funnel, you will get a shitty yield. This is not news, but it bears repeating because it makes all the difference in the world.

LONG LIVE BAALCHEMIST!!

~~~"There's a methyl to my madness"~~~
  
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by scram (Hive Bee)  
  Posted on 11-17-00 12:41  
 
MM, either you got some badass nitro or your friend is doing this in a warm room. I never have had problems with up to 50g al 40ml nitro in a 3 liter FB w/300mm liebig. Its being done at ambient temps of ~10c so maybe this is the reason the condenser never gets warm at all. I believe at this time of the year the 3liter 300mm system could handle 50ml nitro and +60g al. It never has got out of hand, the highest the boiling went to was at most 2/3rds of the height of the round part of the flask. 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by Methyl_Man (Hive Bee)  
  Posted on 11-17-00 16:33  
 
Lucky you!

Of course he has badass nitro, it's 99.7%. What other kind is there?

This is another example of how wildly results and conditions can vary between people. Too bad MM doesn't live in Minnesota---he could just set up in the back yard and do these like crazy out in the 10 Farenheit temps, running a Heet/water mix in the condenser. You midwestern bees, get bizzy with this!!

Here in sunny California we have a sweltering 26C as the room temp. Things heat up awful quick.
~~~"There's a methyl to my madness"~~~ 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by Don_Majic_Juan (Newbee)  
  Posted on 11-22-00 13:12  
 
scram...
   I'm curious...what kind of yields are you getting when doing 50g al / 40ml nitro in an ambient of 10c?
- mama se mama sa ma ma cusa
  mama se mama sa mamacusa 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by scram (Hive Bee / Eraser)  
  Posted on 11-23-00 06:22  
 
Recently....really shitty! So crappy that I'm thinking of retiring. I don't distill so it's a impure matrix of oils among the ketone which by practice I've concluded its only ~30% molar yield from safrol to ketone (If I still remember this correctly). Last sucky reaction used 46 ml of this oil and resulted only 9 grams powder. When things were good it was 75ml of this oil resulting in 21 grams. Roughly speaking 1/3 of the volume of my oil is calculated to grams, so its about 15g per 45ml oil. I haven't done 50g reactions for a while, but once I get my ketone yield up I'm going to attempt it. My highest yield was 27g from 125ml oil but that was a bitch with a 1 liter sep funnel. 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by pmpB_4 (Stranger)  
  Posted on 11-23-00 07:09  
 
that sounds cool baal,
in the last few swinms bee closely monitoring the drip rate to the al breakdown. and is getting 92 outta 100g everytime. he ran some labgrade tone through it and got 112 outta 100 so the labskills are definately a key to the yield! this is using 6000ml fbf with  4 1/2 eggbar, 2 600mm highsurface area condensors and 3-4 drops per second drip rate diden't lose anything out the top. which seems to be a key factor for the yield, also using the bare minimum of meoh helps the reaction alot!
hat's off to mm who set this all in motion!
PmpB_4 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by Osmium (Stonium's / Changer)  
  Posted on 11-23-00 09:31  
 
Sigh...

200g ketone + MeNO2 reduction, done in a 4L flask with THICK Al....

No runaway reaction, plenty of time to add all the ingredients, less Al. But you all heard it before. 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by spric (Hive Bee)  
  Posted on 11-24-00 05:11  
 
What kind of yields are occuring in the busy land of the bees with very quick additions.  Dave tried a 15min addition on 25g scale in 2L with 40cm condensor.  The pressure equalized addition funnel on top then became a condensor after the violence of the reaction.  This was with 200mg (actually 0.2g on the ohaus)HgCl2, which took longer to get started (it was below freezing outside at the time), but did the old volcano on dave.  Pulled 21 g, but lost ~1.5 from recrystallizing.  Something funny happened when trying a second gassing.  Normally all the crystals come out the first time, but this run a second gassing revealed ~7g of piss yellow crystals.  They cleaned up but left a tan tint.
she made a hundred thousand dollars, ended up in federal prison, twenty years for spreading minds 		 
 
 
 
  Subject Re: we need an updated ketone/nitro writeup New   Reply  
  Posted by pmpB_4 (Stranger)  
  Posted on 11-24-00 22:32  
 
swim has gotten good yields with faster addition, as long as the addition wasen't faster than the condensers could handle. just did one with thicker al normal speed addition and a 5 hour reflux and got 47 outta 50. 		 
 

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