Al/Hg Amination Something went wrong.. Maybe?

[DjTime]

SWIM has a question. Has anyone ever started MM's
amination like it's supposed to be done. And came
back an hour and a half later to find that your
nitro/MDP2P/MeOH funnel was still 2/3 there and that
your Al/Hg had already completed it's RXN? Well I
did and I was like OH Shit what the hell did I do.
So I said well fuck I'm already screwed so I just
dumped the 2/3 rest of the mix into the RXN. Well
to my suprise (only my second amination) It started
a reflux that went all the way to the top of my two
400mm condenser's stacked upon eachother. Needless
to say I lost alot of MeOH through the top of them
No problam just added some more. My question is will
I get any product at all Im going to let the mix
stir all night and see what happens tommrow. Has any
bee ever done this before???

[Bandil]

When you say: "Al/Hg had already completed it's RXN?", what do you exactly mean? Was it totally dissolved or just porrage like?

Porrage like is still quite active. The "binding" Al has just been eaten, but there's still tons of active Al left in the mix. So if that was the case, you might be ok.

You might have gotten a somewhat lower yeild due to your impatience in the end, but there should still be quite some product left for you to enjoy. Swim has made the same mistake with LAH reductions running a little dry one time, but the reduction seemed to go ok, with a slightly lower yeild though.

Regards
Bandil

[technology]

YOu may still end up with some product, just hoping that the exothermic reaction in the end from dumping the nitro/meth/saf is enough to fullfill the reaction..

you have already done it, anyway just finish of and look at is as a practice run, if it pulls of then well done..

least you will be careful nxt time..

good luck DJTime

[nitrous351]

Hell ya you got product in there! If you didn't get any from the last 2/3 of ketone, I would say you got some from the first 1/3.
Let me guess: Did you forget to take the stopper off of your addition funnel? Or did you just set the drip rate WAY TOO SLOW? (I am a cheapskate and didn't want to spend the extra $50 for a pressure-equalized addition funnel)
Let me give you some advice: DON'T LEAVE YOUR Al/Hg AMINATIONS ALONE! You can increase yields by learning to match the 'tone drip rate to the amalgamation rate. You will certainly get lower yields by just setting it to drip at 1 drop/second. Don't bee lazy... it only takes about 50 mins. to aminate ~30g 'tone! If you're too lazy to take 1 hour out of your day to pay attention to something that important, maybee you need a new hobbee.
Sorry for the semi-flame... I know you love this as much as the rest of us. Do it correctly though, and you will be sooooo much happier come gas/titration time! peace

[hypo]

"'tone" is bad: acetone or ketone ??

[methyl_ethyl]

Thanks Hypo, there has been quite a bit of slang in the newbee forums lately, I am not sure why as of late ketone has been referred to as "tone" which I have always known as acetone, using such slang may cause some newbees to think they can reductively aminate C₃H₆O + Al/Hg amalgumation = MDMA, in this thread alone tone has been used in the place of ketone, and meth has been used in the place of methylamine HCL.  Maybe I am just being too picky but sometimes it is aggravating trying to decipher slang, and let us not forget that english is not everyones native tongue.  And this is the newbee forum, so there are bees that might not know any better (god help us), I would hate to hear of anyone wasting their methamphetamine because they read on the hive that they could use meth in place of methylamine in a Al/Hg reductive amination.  

[nitrous351]

I'm sorry, I will not refer to ketone as 'tone anymore. However, in my defense, it was very obvious that I was talking about ketone because this is an Al/Hg amination. Acetone is not used anywhere in this reaction. Ketone is... still not an excuse...sorry....won't happen again.

[DjTime]

After SWIM aminated his KETONE, he got a mere 5
shitty grams of MDMA. Note to self NEVER, EVER,
leave amination in progress. Second note to self
NEVER, EVER dump in 2/3 of your KETONE/Nitro
solution in at once or BAD, BAD stuff happens.
Hope Newbee's read this and learn from my mistake
before actually dooing this.

 -peace

[methyl_ethyl]

Five grams of MDMA from a presumed failed synth, I think you are being a little hard on yourself.  This was only your second amination right?  Be thankful you got anything at all.  Of course you never posted your original amounts, I guess I have to assume you followed the write up as written, which I believe you have stated. 
  
     I say good job, you got product babe, now lets work on yield, equipment, and technique....... 

much_love

methyl_ethyl

[DjTime]

Thnaks Methyl_ethyl. Yes SWIM was following MM's writeup
He started with 25G of ketone. I guess your right though
5 grams is better that 0 grams anyday. Deffinetly yeilds
and technique is what I have to perfect now. I'd love to
be getting 23-24 grams from 25 grams of ketone. Hopefully
that will start happining. A new pump is in the works also.
I am a little hard on myself, but I think it's better that
way if I don't keep my self in line the only person who
will, is not the person I'd like to get to know (LE). Welp
thanks for all the words of encouragement, and I'll keep on
keepin' on ME. Peeeeace out.

[spectralmagic]

Heh, SWISM's first successful amination yielded 1.1g from 17.0g ketone...  5% yield, but he was satisified knowing that he *could* do it, and then fine-tuned things...

Always seems to take 3 attempts before SWISM gets a handle on a process...  almost always due to impatience or missing the "little details"...

[raffike]

From raf's very first Al/Hg Raf got 18 grams of salt from 36 grams of double distilled ketone.But he has also got 7 grams of salt from 90 grams good quality ketone.Lately he's been pulling 43-46 grams out of 60 grams of MDP2P.

[methlab]

Ritter says, that one can restart the reaction by throwing in an extra amount of methanol/HgCl2.

[terbium]

Lately he's been pulling 43-46 grams out of 60 grams of MDP2P.
46 grams of salt out of 60 grams of ketone is only a 60% yield. Switch to catalytic hydrogenation and you could be getting more like 70 grams of hydrochloride salt from 60 grams of ketone (90% yield).

[Mercury]

[baalchemist]

Post 53662 (missing)

(baalchemist: "Al/Hg-Nitro kickin up the yield", Methods Discourse)   Baal wants your yields to increase before next semester starts or you're all getting detention!!!!! and a call to your parents may be in order.........