Author Topic: MeOH/pbenz, Al/Hg and sass oil questions  (Read 6408 times)

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Sh0rtTerm

  • Guest
MeOH/pbenz, Al/Hg and sass oil questions
« on: August 28, 2004, 05:28:00 AM »
Hey Bees,
Long time listener, first time caller… or something,

Anyway, I have a couple questions that I can’t find the answer to with TFSE.

First, If one was to dream about a MeOH/p-benz wacker, how would one know it was done? MM says over 9 hrs, BS(in dmf) says 7.5+. Has anybee run spots on this rxn?

It seems that the reflux of CH3OH is a more repeatable and standard condition then BS/Strikes “room temp”. Anyway, Is this 1 hr. addition plus 8hrs. reflux just some bees guess at long enough?

Are there visual clues to the reactions progression?

If one was interested in running spots, since it’s already in MeOH, could we assume this to be acceptable for the chromatography as well?

How about Al amalgam! I keep reading about bees using millings, filings and turnings. Now how are these bees assuring that the Al is pure and not an alloy? All the shops that I have ever been to machine all sorts of alloys on the same machines. Most of the Al used is some sort of alloy. Does this addional copper/mangonese/WTF ever mess with the reaction/amalgamation? Is this one of the secret reasons for the numbers of failures and low yields?

If one was interested in playing around with Al/Hg and Nitromethane(and thicker Al with a reflux and overhead stirring), why wouldn’t one want to reduce the nitro first? Seems to Sh0rtTerm that bees would want the MDP2P addition to be like Fred Durst jumping in the playboy grotto full of drunk, wet playmates. Sexy amine everywhere, ready to hook up!

Oh, while nobee is reading this anyway, has the washes of sassafras prior to distilling fallen out of favor for any specific reason? If my memory was better I would probably be thinking about NaOH removing eugenol or some such shit. Was that all just hype, or are we to be assumed incapable of washes/emulsions and fractional distillation?

abolt

  • Guest
If one was interested in playing around with...
« Reply #1 on: August 28, 2004, 06:56:00 AM »
If one was interested in playing around with Al/Hg and Nitromethane(and thicker Al with a reflux and overhead stirring), why wouldn’t one want to reduce the nitro first?

A smart Bee would add the Nitromethane first. ;)

Oh, while nobee is reading this anyway, has the washes of sassafras prior to distilling fallen out of favor for any specific reason?

Because duistilling Sassafras is now redundant.

See:

Post 459845

(abolt: "The last ever post on freezing out Safrole", Newbee Forum)



bbeeasheets

  • Guest
distilling sassafras is redundant?
« Reply #2 on: August 29, 2004, 03:24:00 AM »
newbie here, getting ready to try first mdma synth from safrole. Abolt stated that distill of sass is now redundant. Does that mean I can skip this step? I was planning on following brightstars method to the letter except i already have the methylamine hcl. Any and all tips would be greatly appreciated.

Tdurden969

  • Guest
You can skip the distillation if you freeze...
« Reply #3 on: August 29, 2004, 02:20:00 PM »
You can skip the distillation if you freeze separate the safrole.


DoctorFeelgood

  • Guest
i prefer distilling it,
« Reply #4 on: August 29, 2004, 04:25:00 PM »
it goes much faster it's a wya to learn how to distill correctly. producing really pure mdma can not be done without distilling, so learn it. it's a standard setup which you will have to use during following stages, e.g. mdp2p after buffered performic, mdma freebase distilling to remove higher boiling impurities, ...

abolt

  • Guest
More white noise
« Reply #5 on: August 29, 2004, 10:19:00 PM »
producing really pure mdma can not be done without distilling, so learn it.

Yes, but producing really pure Safrole can be done without distillation.


Snakebyte

  • Guest
Your wacker will be done when it goes back to...
« Reply #6 on: August 30, 2004, 08:05:00 PM »
Your wacker will be done when it goes back to room temp which is usually around 7 hours total for swim but an extra few hours will not hurt if your not sure.  Swim also uses alumimun turnings and he prefers these because his amalgamation is so easy to control, gets the best yeilds and there's no pissing around cutting up foil.  He doesn't know if his turnings are 100% aluminum but he knows there are no flakes left in the end.  Lastly, swim has froze his sassy a few times which worked well but he still prefers good old fasion distillation to get clear colorless safrol.


Sh0rtTerm

  • Guest
But for the wacker in methanol, it goes to...
« Reply #7 on: September 08, 2004, 05:37:00 AM »
But for the wacker in methanol, it goes to room temp when you turn the heat off. How gentile is palladium and p-benz? P-benz sure doesnt seem to me like something notI would want refluxing away with mdp2p any longer then needed.

Does anyone know about the aluminum alloys effects on amalgamation?

Snakebyte

  • Guest
My freind's done wacker in both methanol and...
« Reply #8 on: September 09, 2004, 10:34:00 PM »
My freind's done wacker in both methanol and DMF and the flask contents do not go back to room temp with either after heating unless you are heating until near the end of the reaction.  In fact, you don't even need heat to for the reaction to push forward and I would suggest trying it without heat to see if your contents even heat up at all.  It might take 4 hours but it should and if it doesn't, it could mean your catalyst or a reagent is not good enough.


Sh0rtTerm

  • Guest
So should the meoh pbenz wacker be done with...
« Reply #9 on: September 10, 2004, 08:00:00 AM »
So should the meoh pbenz wacker be done with heat or without? It seems that heating to ruflux is a real point of MM's synth, but all the old posts about meoh dont mention refluxing or external heating. I dont think any of the dmf wackers have mentioned external heating. Is MM alone on this heating deal? Has anyone done it back to back with a meoh wacker, refluxing vs no heating and compared yields?

XrLeap

  • Guest
For DMF, there is no need to heat, the ...
« Reply #10 on: September 10, 2004, 08:29:00 PM »
For DMF, there is no need to heat, the reaction itself is exothermic(sp?). You can try adding all in the flask/container, without H2O. The mixture's temperature will not rise, but with H2O, it will rise above 50C.


pooky

  • Guest
Just distill the stuff..
« Reply #11 on: September 14, 2004, 04:19:00 PM »
P used to do very careful freeze purifying of saf,and in Methyl man's benzo wack would get back 90 to 100g double distilled ketone.No matter how slow it took to freeze(days) and how many times (4 or 5)and how dry the 2 inch crystals were,it still smelled "sassy" and had a yellowish  tint.
When P started distilling again,the returns immediately jumped to 120 to 125g with the same supplies unchanged.Distilled saf is water clear and has no sassy smell...period,end of story.
Start distilling,and keep an eye on it while you surf porn or watch TV.When the temp goes up a few degrees,stop.If you want, put the dark brown remainder in the freezer and see if any more crystallizes over a week or 2.


Sh0rtTerm

  • Guest
So what about the demon eugenol?
« Reply #12 on: September 15, 2004, 06:06:00 PM »
So what about the demon eugenol? Do those that distil do any washes first? It used to be the rage to hit it with water, then NaOH solution(10%? I cant remember), then more water, then put it in a big beaker and run it to 120C with strong stirring to remove the water, then in the vac distilling rig. What colums are beez using now? I saw somewhere(Rhods page? here?) of someone just doing a simple distilation with no column. Seems dumb. If you want pure... Also, better to practice with saf in sass then mdp2p.

That isn't two cents. It's lira...

abacus

  • Guest
I did it at atmospheric
« Reply #13 on: September 16, 2004, 02:47:00 AM »
Freezing may be the way to go, but to answer your specific question.

Never washed, but did follow this procedure.

Used standard lab glassware, no column just plain stillhead. 

Dissolved sassy in equal volume of denatured ethanol
Added enough water so that safrole seperated from solution (75% volume of starting sassy)

Seperated mostly safrole from alcohol/water layer

Set up for atmospheric distilling
Heated up and discarded all distillate below 220DegC
Continue heating and distilled the safrole coming over from 230DegC to about 240DegC or when distillation stops.

Yields safrole normally over 90%.

Left with small amount of undistilled oils in the flask

You will need a very good heat source to do this (heating mantles are excellent for this), and the ethanol rinse may be redundant.

You don't need to vacuum distill safrole, wheres you normally do need to vacuum distill isosafrole, ketone, freebase (especially) at much lower temperatures.

I hope this helps

Abacus

Snakebyte

  • Guest
I don't know what type of sassy you are using...
« Reply #14 on: September 16, 2004, 12:21:00 PM »
I don't know what type of sassy you are using but in Swim's experience 1x simple distillation gives clear colorless safrol that works great in a wacker.


XrLeap

  • Guest
For crystallisation of safrole, you keep the...
« Reply #15 on: September 16, 2004, 01:30:00 PM »
For crystallisation of safrole, you keep the sassy at 10C(0C or -20C is bad), add in seed obtained from distillation. Throw in the seed which is big enough, that will not dissolve all in the solution. The xtallisation will start slowly, collect it 2 days later. You got crystal clear safrole or safrole crystal clear or clear safrole crystal. ;)

there will be yellow/brown liquid left unfrozen. decant them, and maybe you want to wash the crystal with some alcohol to get rid of the brown oil.

Keep your still for other use, eg ketone, iso.....