Author Topic: Thick Al and nitro success  (Read 914 times)

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abacus

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Thick Al and nitro success
« on: October 08, 2001, 04:06:00 AM »
Finally after very low yields with Al foil, SWIM has had a breakthrough using 300 micron thick aluminum foil and nitromethane.

SWIM produced his ketone via the modified performic and all appeared to go by the book except when distilling the ketone,  which started coming over at 135 Deg C with a water aspirator vacuum source, gradually climbing and finishing around 190 Deg C at which time it turned to crude.  So swim wasn’t too sure about the quality of his ketone.

Successive animation attempts using thin foil yielded at best 5 gms of honey per 30 grams of ketone and SWIM was losing all hope that he could achieve a decent yield as he had no idea what the problem was, until he tried the following.

Aluminum Foil Testing

SWIM tested various aluminum foils, pie plates, BBQ trays etc to see if they would be any good by simply cutting up a few squares and throwing them into a small beaker with some ethanol, adding a pinch of mercuric chloride, waiting a few minutes then adding a few mls nitromethane.  In some cases nothing happened which indicated this was not good foil to use, and in a few other cases the foil immediately began to break down, the flask heat up until boiling and methylamine being produced.

So SWIM was keen to test some recently acquired soft Aluminum flashing which is 0.3 mm thick to see how this would fair, and sure enough the thick aluminum immediately amalgamated and reduced nitromethane to methylamine almost as fast and as hot as the thin foil.  

SWIM was now really curious to see what would happen using when using this thick sheet in the nitro/ketone al/Hg animation.

Reaction

SWIM cut up 27gms 0.3 mm thick aluminum flashing into 1cm square pieces and placed in a 2L 2 neck FB flask with 750 ml methanol and 20 ml dH20.  An impromptu overhead stirrer was added through the side pocket but promptly broke on testing so the overhead stirrer was abandoned in favor of a small stir bar.

The stir bar wouldn’t stir the aluminum but SWIM wasn’t going to stop to fix the overhead stirrer.

Around 100mg mercuric chloride was added, swirled by hand an let rest.  SWIM’s Graham condenser was added to the flask and a mixture of 25ml supposed ketone of unknown quality, 20ml nitromethane (purified by re distillation of 100% hobby shop stuff) and 50ml methanol was mixed into a dripping funnel.

After 10 minutes, another pinch of mercuric chloride was added followed by a quarter of the nitro/ketone mix from the dripping funnel now in the side arm of the flask.  SWIM was expecting this to really kick start the reaction but only noticed some aluminum starting to break down and no noticeable temperature rise.

Surprised by this SWIM added all of the ketone/nitromethane mix and another pinch of mercuric chloride.  

Within 4 minutes the reaction was well under way and refluxing hard.  Stirring was achieved by hand swirling the flask for a few seconds every few minutes or so.  The reflux rate was unnerving, but not as strong as SWIM had seen when using thin foil.

After another 10 minutes, SWIM added a few more mls nitro down the condenser just to be sure.  After 25 minutes of periodic hand swirling and resting, enough of the aluminum had broken down so that the stir bar would stir the mix.

SWIM relaxed and let the reaction reflux on its own for the next hour or so with a bit of heat added.  After 2 hours some aluminum was still resting in the flask so a few mls nitro was added which produced a bit more methylamine and kick started a small reflux and then the whole mix was stirred until at room temperature.  This was around 5 hours after the reaction started. 

The thick blue grey sludge with left over aluminum pieces was poured through a strainer into a 3L beaker to remove the leftover aluminum.  750 ml 35% NaOH was added followed by 400mls xylene and stirred for 20 minutes.  This was decanted and collected and then another 2 portions of 150 mls of xylene was stirred in the beaker for 10 minutes and separated.

The combined xylene was washed with 300ml 1M HCL.  The aqueous phase was separated and filtered and then basified with 25% NaOH.  When enough NaOH was added SWIM couldn’t believe his eyes to see about 20ml yellow oil fall out of solution to the bottom of the separating funnel.

200 mls xylene was added to dissolve the oil and then separated off.  The xylene was dried over 25 grams magnesium sulfate for 30 minutes, filtered and gassed.

SWIM thought he was dreaming to see the flask turn almost solid like ice cream. 

The crystals were collected on filter paper and washed with dried acetone.  The xylene gassed once more, the crystals collected and washed to yield a total of 24 grams snow white MDMA ready for recrystallization

SWIM is over the moon considering no need for an overhead stirrer, don’t have to worry about dripping the ketone /nitro mix in slowly, and can throw the aluminum foil away.
 

cilliersb

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Re: Thick Al and nitro success
« Reply #1 on: October 08, 2001, 06:09:00 AM »
Just one question on the Modified Performic. After the NaOH wash, did your organic layer turn milky and become very difficult to extract? Oh yes, and how long did your Brine wash take to seperate?

My ketone also had some problems with the temp where stuff started boiling, but this is supposed to happen. The reason for distilling is that we are trying to remove impurities. First distill your sassy oil and make a note of where it comes over with pump Vac. Now calculate the Vac. that your pump generates and make a note (you know the boiling point of sassy @ atmospheric). Knowing your Vac. you can calculate the boiling point of your ketone at this Vac. Re-distill your ketone and keep no more than a 15C fraction from the calculated boiling point to 15C higher.

Your earlier failures may have been due to dirty ketone. Ass long as there's aluminium the reaction should run fine with the proper control of temp and addition rate.


abacus

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Re: Thick Al and nitro success
« Reply #2 on: October 08, 2001, 01:45:00 PM »
There is no NaOH wash with the modified performic, never done one.

Also SWIM is convinced the previous low yields was due to aluminium foil, and not the ketone, as SWIM used some of the the SAME batch of ketone with the .3 mm Al to finally get a good result.  Whereas using this ketone with thin foil produced very low yields.

The batch in question was the stuff collected from 135Deg right up to around 190 Deg.  The fact that SWIM just got 24g honey from around 29g (25ml) of this stuff means its good enough for this bee.

baalchemist

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Re: Thick Al and nitro success
« Reply #3 on: October 10, 2001, 12:04:00 AM »
Thats usually a newbee sign these days Abacus, you know> change all the parameters and combine 3 different synths w/3 whims because they feel right & cant figure out why shit still isnt up to par kinda shit ;) . Congrats with the flashing, that works great especially if youre going Osmiums route for large-scale kingbee style.

GODISNOWHERE

abacus

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Re: Thick Al and nitro success
« Reply #4 on: October 10, 2001, 04:10:00 AM »
SWIM was quite confident the flashing was the answer, so he cut up some more flashing and went at it again.  This time he shortened the reaction time to about 4 hours (due to impatience only) and noticed more unused al left over, used an unkown solvent for extraction and gassing to end up with 10 grams honey from 25 ml same ketone as before.

Looks like plenty of work to do yet and SWIM has learnt adding new variables wasn't very smart after 1 success!!!!!!





foxy2

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Re: Thick Al and nitro success
« Reply #5 on: October 10, 2001, 06:57:00 AM »

used an unkown solvent for extraction and gassing




Why????
Why fuck your reaction up on the easiest step?


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Antibody2

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Fucking oven liners!!
« Reply #6 on: October 10, 2001, 11:41:00 AM »
I hear ya about that voodoo aluminum. I also have experieneced unamalgamatable foil, or even worse partial-unamaglgamatable foil cuz that sux you into starting the rxn!

only experienced the problem with oven liners, they must have some coating that screws with the amalgamation.