Author Topic: failed amalgam -- wondering if anyone has seen this before. (Read 330 times)

pbinteger · « **on:** January 19, 2013, 08:43:41 PM »

Hello Vesp

So I ran a reductive Hg/Al amination last night. I followed the exact same procedure that I did last time which was very successful. However, I noticed that more of the aluminum than I would have expected was left undissolved at the end, and the reaction never got as vigorous as the last time. So when I based it out there was a crazy vigorous reaction as all that aluminum dissolved. I smelled methylamine though so I figured everything was fine. Also the color looked good a nice blue grey chowder. I worked it up as written and with the same method as last time. I noticed that my first Toluene extract was yellow which was very different than last time. Last time everything was clear. As I washed the toluene with water and brine it did clear up but not much -- it remained yellow. When I went to gas the toluene it turned bright blood red and no crystals came out. I'm calling this a failure but I'm not exactly clear on the possible mechanisms of failure for this reaction.

Could it be unreacted isosafrole that I didn't catch in fractional distillation of mdp-2p? If so, would acid / base extraction give me the pure freebase? It seems that even if there was unreacted iso in the mix -- the freebase would have converted to hydrochloride upon gassing it with dry hcl(g).

Any insight would bee appreciated.

_Pbint_

fishinabottle · « **Reply #1 on:** January 19, 2013, 11:08:16 PM »

Albeit the fabric of information is thin I think it is legit to say that your ketone was most probably not good. I give it a 98% probability to be exactly this.

/ORG

pbinteger · « **Reply #2 on:** January 20, 2013, 12:19:31 AM »

That would make sense, but this was the rest of the SAME ketone that I used in the first 50g reaction that produced ~40 g of pure white MDMA -- excellent purity....

I kept it in the freezer... perhaps some impurities (isosafrole) had settled to the bottom of the jar?? Even that doesn't make sense because the isosafrole would have frozen -- and this remained a neon green sweet smelling oil at -10c.

I think I'm going to convert this next batch of MDP2P to the bisulfite adduct.

so weird...

Sneak · « **Reply #3 on:** January 20, 2013, 12:49:01 AM »

Gutted for you!

Sounds strange indeed.

How much gas went into it before this happened?

pbinteger · « **Reply #4 on:** January 20, 2013, 06:08:19 AM »

It's times like these where I needs me some spectral analysis equipment that works

fishinabottle · « **Reply #5 on:** January 20, 2013, 05:36:15 PM »

As said you did not provide information on the reaction itself except that it worked another time.
You say there was not as much reacting as used to be.
So I deduce there was not enough to react and this leaves it with the ketone or the aluminium amalgam. Now you say the ketone was the same and as you describe it was good.
Leaves the aluminium. Same Al? Same amount of the same Hg salt? Are you sure amalgamation was sufficient? Why are you sure?

If the answer is not to find here a spektrometer wont help you either as then only the hand of god is left, who wants you to leave your evil ways of drugs and get reborn. As ex-president Bush how this is done he knows.....

/ORG

pbinteger · « **Reply #6 on:** January 20, 2013, 09:29:42 PM »

LOL!

Jesus was an alchemist...

I used the same aluminum, prepared in the same manner.
I used ACS grade Mercuric Nitrate in the same molar ratios as the previous reaction.
I do believe, the lower solubility of the Mercuric Nitrate in MeOH, left perhaps a bit too much of the undissolved salts on the walls of the boiling flask I was using to stir the methanolic solution before it went into the reaction vessel. I noticed that after the reaction had already begun.
It did seem that the amalgamation petered out too soon, unlike last time. Can the headroom of the reaction vessel in relation to the volume or scale of the reaction mess things up? I used a 5L round bottom for this scale and the reflux never became very vigorous. I could see the reflux ring near the top of the flask but never really too much into the cold condenser. Does this reaction need a lot of reflux to run smoothly?

These are not drugs -- these are empathogens

Ex-president bush probably does cook meth in his secret underground lair.

_Pbint_

Wizard X · « **Reply #7 on:** January 21, 2013, 01:12:21 AM »

The scenario: 16 Uni chemistry students (2nd year) performing a metal reduction (Al/Hg) synthesis of Cadaverine. All used the same LR grade reagents, all had the same lab equipment and synthesis procedure. 9 failed, and 7 were successful.

I think you can see where this is going...

d1ssonance · « **Reply #8 on:** January 21, 2013, 05:48:37 AM »

How is your source of stirring?

In my experience overhead stirring is needed, magnetic stir bars dont work in the rxn.

Also how did the aluminum look? Was it broken down, or still shiny and balled. If the former then you didn't allow amalgamation to proceed for long enough.

Next time it happens try heating it a bit to the point of reflux and see if that jump starts the reaction.

Also you could try distilling your solvent off to see what you're left with. If you think your ketone is good then it should remain if no rxn. There also may be a chance that your atmosphere was too humid and you'll distill the MDMA freebase, which wouldnt be a bad thing at all.

fishinabottle · « **Reply #9 on:** January 21, 2013, 06:14:00 AM »

Did you reflux it for some hours after it had ceased to go by itself? And how much mercury nitrate did you actually use? Amalgamation done in the vessel or seperately? Usually the nitrate is just fine, but that knowledge refers to amalgamation in water....

It's the hand of god, repent!

@WizardX: If this happened in Australia I bet from the 7 who succeeded were at least 6 from India...

/ORG

PS: d1ssonance, the too humid atmosphere is a good one taking into account that there is a lot of water in the reaction from start, or is humidity another kind of water then the dihydrogen monoxide we know?
Besides overhead stirring being superior in almost all reactions in special when the vessel exceeds a certain limit, magnetic stirring works well in an Al/Hg, whereby the kind of Al one uses is of importance. With aluminium shavings there is little issue, but with sheet or foil it may look different.

The ketone will probably not be recovered as I am afraid it reacts anyways. If not with methylamine and aluminium as this option is not given for any reason it may well decide to condense a little bit with itself and then a little bit more and so on. The different high molecular weight polymeres may have interesting properties but they are not anymore whats wanted and needed. I would reer from recovery operations as this will IMHO end in just more frustration (and heaps of time and solvents wasted).
To kickstart when its more or less running heat wont suffice, heat and half a gram of mercury salt sometimes do.

pbinteger · « **Reply #10 on:** January 21, 2013, 05:56:52 PM »

@WizardX -- I know I need to improve my technique -- every time I run a reaction I try to identify ways to improve.

I've been using a large 3inch stir bar and it's worked well.. I was always able to stir vigorously. I need to get set up with overhead stirring.

Also how did the aluminum look? Was it broken down, or still shiny and balled.

It was almost all broken down but there was maybe ~6-8 grams of aluminum that was still shiny / balled all the rest ~26g was completely broken down.

I refluxed for 3 hours after -- I did apply heat but not some extra mercuric salt. I thought about that, but was unsure of the consequences

I used 580mg of Mercuric Nitrate for 33grams of Ketone. The same ratio as last time which was a great success where I used 880mg for 50g of ketone.

d1ssonance · « **Reply #11 on:** January 21, 2013, 11:19:45 PM »

Quote from: fishinabottle on January 21, 2013, 06:14:00 AM

Did you reflux it for some hours after it had ceased to go by itself? And how much mercury nitrate did you actually use? Amalgamation done in the vessel or seperately? Usually the nitrate is just fine, but that knowledge refers to amalgamation in water....

It's the hand of god, repent!

@WizardX: If this happened in Australia I bet from the 7 who succeeded were at least 6 from India...

/ORG

PS: d1ssonance, the too humid atmosphere is a good one taking into account that there is a lot of water in the reaction from start, or is humidity another kind of water then the dihydrogen monoxide we know?
Besides overhead stirring being superior in almost all reactions in special when the vessel exceeds a certain limit, magnetic stirring works well in an Al/Hg, whereby the kind of Al one uses is of importance. With aluminium shavings there is little issue, but with sheet or foil it may look different.

The ketone will probably not be recovered as I am afraid it reacts anyways. If not with methylamine and aluminium as this option is not given for any reason it may well decide to condense a little bit with itself and then a little bit more and so on. The different high molecular weight polymeres may have interesting properties but they are not anymore whats wanted and needed. I would reer from recovery operations as this will IMHO end in just more frustration (and heaps of time and solvents wasted).
To kickstart when its more or less running heat wont suffice, heat and half a gram of mercury salt sometimes do.

ZING, WOW GOOD ONE! HOW WITTY. DIHYDROGEN MONOXIDE HAHA....

I meant in his gassing set up. You know, when you salt out a molecule from its freebase? There are numerous sources that cite trouble with gassing this way (spiceboy mentioned it many times in his post, and also stated he preferred titration to salting the freebase.

pbinteger:
Never used Mercuric Nitrate for an amalgam, but using mercurous chloride I usually wait almost 30-60 min longer for amal than with mercuric. I usually use some heat to speed it up as well.

Wizard X · « **Reply #12 on:** January 22, 2013, 03:12:09 AM »

Quote from: fishinabottle on January 21, 2013, 06:14:00 AM

@WizardX: If this happened in Australia I bet from the 7 who succeeded were at least 6 from India...

Anglo-Saxon, Asian, Middle-Eastern.

newbiechem · « **Reply #13 on:** January 22, 2013, 04:11:15 AM »

its simple....

its about the timming for the almagnization of aluminum before you add ketone.....
sometimes takes longer for the Al to react with the HG....

wait at least 30 minutes, 40 to be sure, lots of bubles, aluminum with dull color not shiny....then you good to go....

peace

Whale · « **Reply #14 on:** January 22, 2013, 03:49:54 PM »

If you were to wait would there may be a problem with all of the ketone turning into precious freebase?

d1ssonance · « **Reply #15 on:** January 23, 2013, 05:13:17 AM »

Quote from: %1 on January 22, 2013, 03:49:54 PM

If you were to wait would there may be a problem with all of the ketone turning into precious freebase?

If you're talking about the previous poster i'm pretty sure he's talking about waiting for amalgamation to proceed.

fishinabottle · « **Reply #16 on:** January 23, 2013, 05:36:22 AM »

Well you used a lot of solvent in the amalgamation IIRC, that should be just enough to cover the aluminium and two fingers more, its about concentration.

The nitrate works just fine I never saw any difference to the chloride. Stirring, not permanently but some good bursts helps.

What everybody here is talking about amalgamation taking 30 minutes is incomprehensible to me, what are you using? Solid blocks of aluminium?
When real pure aluminium is used 99,99% and in a usable form like shavings, amalgamation in water takes 3 minutes maximum. Then it has to be washed quickly with icecold water to remove excess mercury and stop it as it gets already wild.
This refers to methylamine/ketone reactions, in nitromethane/ketone amalgamation is done in situ to slow it down, same in P2NP reductions to the amphetamine.
But thats here MeAm/MDP2P if I got it right? Then separate amalgamation is the way to go.

I am under the impression that the quality of the aluminium got neglected by many if not the most and problems arise logically out of this.
Foil is a crutch. Get real, pure Al, it is available and even if you buy an ingot, two hours with a power drill are not to much work to invest in my world.

/ORG

PS: And anyways, if you believe for whatever reasons that the chloride salt of mercury will be your salvation and the nitrate is the evil bringer of defeat, well if you believe this albeit its complete nonsense, but most religious believes are just this and thats religious as without any foundation by facts, so you can nevertheless get to your holy grail without much effort.
Just adding HCl to the nitrate will schwuppdiwupp convert it to the chloride. Same as adding a pinch of a nitrate to a mixture of Hcl and mercury will amalgamate any Al present like mercuric chloride. or the simple reason that thats exactly it.

Good Al looks like this example

newbiechem · « **Reply #17 on:** January 23, 2013, 06:51:01 AM »

well i will say again!!!

as a matter of fact i use not 99.99999999% aluminum .... i rather buy some at the supermarket
what i saw was reynolds super heavy duty AL foil its much thicker probely 98-99% "pure aluminum", and YES im not a chemist like many over here, but saw this happens.
3 minutes i dont even have courage to put precious ketone into it....FAIL every time. unless you have like 400mg of mercury wich i also have no balls to put that much into lets say 50gr aluminum. maybe if you put 400mg of mercury your aluminum will react in 3 minutes, or maybe using regular thin aluminum foil.....or "real aluminum"which i only heard at the hive, and i dont remember being that good.
maybe your react in 3 minutes because its in water not methanol, i dunno if this would afect.....also why in the name of any God would you react your aluminum, then take it out and wash it?

correct me if i am wrong but doesnt the skin ABSORVE THE MERCURY IN WATER?? very danger if any just touchh you skin??? thats NOT practical AT ALL, even worst when you fucking around with mercury, and mercury that your skin will absorve!!!!

...maybe im just crazy.

so once again the guy probely dont have 99.999999999% aluminum like everyone, so MAYBE its does take longer for almaganation, since aluminum foil tends to have some coating (no! it does not afect anything AT ALL) just make sure the amalganation its happening, if you doing with fish and not nitro even easyer cuz you dont need the exact timing, just cant be before the whole thing is bubling and you sure amalgantion its taking place.....stirr every 10 minutes (if you go this way and not 3 minutes), around 30 should be good, if you using 150-170mg of mercury. you must learn the amalganation point, sometimes goes a lil faster some times a lil slower.
well, said that because seen this problem happen before, try do to a test make 2 runs one with 5 minutes amalganation and the other with strong amalganation maybe 30 minutes (depending how much mercury). and bring us back the answer

i think if you starting now you will see that most timing is useless, you need to learn how the reaction works so you know when its the right time for everything... no matter anyone says how long it takes....as you can see ones takes 30-40 minutes others take 3 minutes

but i am sure thats your problem!! stirr the mercury well in the methanol untill everything siddolved, then make sure the amalganation took place!!!! no problemo if pass a lil bit since you using fish hehehe

hope was some help.....
bring back results
peace!!!!

fishinabottle · « **Reply #18 on:** January 27, 2013, 04:17:54 AM »

Was using foil and sheet for a long time before I discovered the pure shavings and decided to give it a try. And I was astonished and pleased in how much positive difference it makes.

I bought it somewhere everybody can buy it without any problems, it is not from a lab supply house you know?

Nevermind. Getting pure reagents can be easy and they make life much easier. Sounding from your post foil or whatever you use makes things pretty difficult and I only missed the additional use of magic for rationale is only little in your rantings, but religious belief plenty.

I enjoyed reading a genuine confused tweaker post though, they got rare.
Tweak on!

regards
/ORG

Author Topic: failed amalgam -- wondering if anyone has seen this before. (Read 330 times)

pbinteger

failed amalgam -- wondering if anyone has seen this before.

fishinabottle

Re: failed amalgam -- wondering if anyone has seen this before.

pbinteger

Re: failed amalgam -- wondering if anyone has seen this before.

Sneak

Re: failed amalgam -- wondering if anyone has seen this before.

pbinteger

Re: failed amalgam -- wondering if anyone has seen this before.

fishinabottle

Re: failed amalgam -- wondering if anyone has seen this before.

pbinteger

Re: failed amalgam -- wondering if anyone has seen this before.

Wizard X

Re: failed amalgam -- wondering if anyone has seen this before.

d1ssonance

Re: failed amalgam -- wondering if anyone has seen this before.

fishinabottle

Re: failed amalgam -- wondering if anyone has seen this before.

pbinteger

Re: failed amalgam -- wondering if anyone has seen this before.

d1ssonance

Re: failed amalgam -- wondering if anyone has seen this before.

Wizard X

Re: failed amalgam -- wondering if anyone has seen this before.

newbiechem

Re: failed amalgam -- wondering if anyone has seen this before.

Whale

Re: failed amalgam -- wondering if anyone has seen this before.

d1ssonance

Re: failed amalgam -- wondering if anyone has seen this before.

fishinabottle

Re: failed amalgam -- wondering if anyone has seen this before.

newbiechem

Re: failed amalgam -- wondering if anyone has seen this before.

fishinabottle

Re: failed amalgam -- wondering if anyone has seen this before.