Author Topic: Alternative To Gassing Ideas?  (Read 6859 times)

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TheBlindGenius

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Anything more accurate than that?
« Reply #60 on: October 28, 2002, 06:34:00 AM »
Like maybe a Karl Fischer titration or something, I know it's used to measure moisture content but don't know much else about it.  Anyways, I'm gonna give it a crack using the inverted funnel maybe later this week since no one seems to have any major objections to that approach.  Anyone want to give me some info on the KF titrations?  I see in my catalog a Denver Instrument Cuolometric Titration Controller for over $2000 that is for KF titrations.  Does KF titration have to be that expensive?  Damn!  :P

TheBlindGenius

  • Guest
Another way
« Reply #61 on: November 25, 2002, 08:02:00 AM »
How is the 5-6 N HCl/IPA from acros made? By gassing!!
Adding CaO to wet HCl in IPA would be a good, but expensive, way to get CaCl2.
Why don´t you simply follow more experienced bees advice and devote one, just one, day to make your stock solution of HCl in whatever-solvent?


There is another way that does not involve any gassing at all.  Dissolve acetyl chloride in cold anhydrous methanol. 

CH3OH + CH3COCl --> HCl + CH3COOCH3

The byproduct is methyl acetate.  Perhaps there is some way to remove it, or maybe it does not interfere with our desired reaction?

Osmium

  • Guest
Solutions of hCl in alcohols aren't inert, they ...
« Reply #62 on: November 25, 2002, 03:13:00 PM »
Solutions of hCl in alcohols aren't inert, they will slowly react with each other producing the alkyl halogenide.

I'm not fat just horizontally disproportionate.

TheBlindGenius

  • Guest
But does that matter?
« Reply #63 on: November 25, 2002, 05:46:00 PM »
Will the alkyl halogenide (alkyl halide?) react w/ MDMA/MDA/2CB freebase at all?  Also, how long does this take to happen?  I was under the impression that a lot of people gas their solvent and store it until they have freebase, which can be a long time.  That's why I like this method, because you can do it on the spot at any time without setting up a gassing apparatus.

Osmium

  • Guest
> But does that matter? Yes, sometimes it ...
« Reply #64 on: November 26, 2002, 12:48:00 AM »
> But does that matter?

Yes, sometimes it does. I've seen examples, e.g. a report by some industrial chemists who tried to prepare a methylester by saturating the methanolic solution of the compound to be converted with HCl gas. While this reaction apparently gave excellent yields and purity in rather short time when done small scale, it didn't work very well when scaled up to industrial proportions, leaving an almost impossible to clean up and difficult to filter mixture after several hours reaction time. Nobody could explain the differences until they found out that the HCl converted some of the MeOH into MeCl which reacted with another site of the molecule, producing impure shit.

> Will the alkyl halogenide (alkyl halide?) react w/
> MDMA/MDA/2CB freebase at all? 

Yes.

> Also, how long does this take to happen?

The side reaction starts as soon as you stick the gassing tube into the alcohol.

> I was under the impression that a lot of people gas their
> solvent and store it until they have freebase, which can
> be a long time.

I wouldn't store it for too long. I have no details, but I assume that MeOH and EtOH are much more perceptible to this kind of side reaction than e.g. IPA.

I'm not fat just horizontally disproportionate.

TheBlindGenius

  • Guest
OK, so you said sometimes
« Reply #65 on: November 26, 2002, 03:10:00 PM »
What would the reaction be if you had an amine freebase such as MDMA and an alkyl halide in solution?  What would the product be?  Also, how about methyl acetate, would it react with an amine freebase?  If so, what would the product be?  MDMA acetate?

Rhodium

  • Guest
Methyl acetate may acylate MDMA to N-acetyl-MDMA, ...
« Reply #66 on: November 26, 2002, 05:27:00 PM »
Methyl acetate may acylate MDMA to N-acetyl-MDMA, and methyl chloride may alkylate MDMA to N-methyl-MDMA (N,N-Dimethyl-MDA).

TheBlindGenius

  • Guest
Distillation of HCl/MeOH
« Reply #67 on: November 26, 2002, 09:47:00 PM »
OK, here's another question.  What would happen if one were to distill HCl/MeOH solution?  Would the HCl/MeOH come over together, or would the HCl come over first then the MeOH?  I know that NH3/water comes over first the NH3 then a NH3/water solution (at least that's what we did in analytical chem when analyzing ammonia content in an unknown).  The reason I ask is maybe methyl acetate can be removed by distillation?

RoundBottom

  • Guest
a tale of two salting methods
« Reply #68 on: December 03, 2002, 01:45:00 AM »
in the interest of... well... me, a test was performed to determine which yield better results, gassing or titration.  less than expected results has become a trend lately, and has cast a dark shadow over the lab.  now, before you yell NOOB!, drying and gassing are not new experiences hereabouts, and proper yields have been accomplished regularly in previous attempts.  investigations were made, apparatus cleaned and replaced, but to no avail; the spate of poor gassing yields continued.  so, this experiment was attempted to decide if methodology should be changed.  titration has never been attempted before, and it was decided this was a perfect opportunity to try it out.

PREFACE: the Al/Hg run in question was run as per

Post 343969

(RoundBottom: "Os/BS AlHg MeAm Amination writeup", Methods Discourse)
, and at least 50g was expected from this particular attempt.  upon final drying of toluene, the volume of toluene was measured (about 650mL), and split into 2 equal halves. 

the first half was gassed immediately, as per usual, and a disappointing 16.1g was recovered where ~25g was expected.  the toluene was gassed and vacuum filtered 6x, until, on the 6th gassing, there was no more precipitate.  the standard H2SO4 on HCl generator with inline drying tube (filled with indicating dri-rite) was used.

the second half was left overnight and attended to the next afternoon.  a 5% HCl solution was made (using muriatic acid, 31.45%), and slowly dripped into the beaker containing the toluene while the toluene was stirring on HIGH.  the pH was checked after every eyedropper squirt (~1mL of 5% HCl).  after many, many, many! squirts (got bored, lost count after about 30) the pH measured 3.5/4.  the contents of the beaker were placed in a 500mL sep funnel, and allowed to separate.  the bottom, aqueous layer (which had turned dark blue, possibly from the pH strip indicator?) was drained into a clean pyrex dish (the toluene was kept to make sure nothing was lost) and left to slowly evaporate the H2O.  after a couple days the water had (mostly) evaporated, and a large, flat crystal sheet was on the bottom of the dish.  it still had a dark blueish hue.  this was scraped off, broken up and put in boiling acetone for 20 minutes, then filtered again.  after drying, 25.3g clean salt was recovered.

even for a first attempt, titration seems to have won a new convert.  a difference of almost 10g was achieved, and a whole lot of recovered toluene is going to be titrated for hidden remainders.

gassing stinks, is tedious, dirty, and can be dangerous.  it also requires anhydrous conditions, which, if not achieved, may scuttle your yields.  gassing's main advantage is it is quick.

titration has the advantage of doing away with anhydrous conditions, but it takes a while to evaporate the water and get crystals. 

if you have the opportunity, give this experiment a try.  the results may surprise you.

next up, sassy distillation vs. crystalization.

Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)

Osmium

  • Guest
Your results with gassing would have been much ...
« Reply #69 on: December 03, 2002, 05:29:00 AM »
Your results with gassing would have been much better if you had used less toluene, evaporated the toluene after the gassing and collected/processed the leftovers.

You also have to consider that your titrated product isn't anhydrous like the gassed product, it contains water of crystallisation. 100mg of each contain different amounts of active ingredient.

I'm not fat just horizontally disproportionate.

RoundBottom

  • Guest
> gassing would have been much better if you ...
« Reply #70 on: December 03, 2002, 01:10:00 PM »
> gassing would have been much better if you had used less toluene

interesting.  many have wondered what the proper amount of toluene is to extract freebase.  and it is recommended to then reduce the volume of toluene to facilitate gassing?  does this concentrate the freebase making it easier to receive the HCl?

> titrated product isn't anhydrous like the gassed product, it contains water of crystallisation

is this true after boiling briefly in acetone, filtering, and drying again?  after doing this, the product has the same fluffy appearance as gassed product.

thanks for your insight, mr o.

Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)

hCiLdOdUeDn

  • Guest
Cool RB!, Swim has tried gassing and it works OK, ...
« Reply #71 on: December 03, 2002, 01:45:00 PM »
Cool RB!,

Swim has tried gassing and it works OK, but yields arent as good as one might like. Also setting up for gassing is tedious. I will also try your titration method!

Sink or SWIM

Osmium

  • Guest
Attention sarcasm ahead
« Reply #72 on: December 03, 2002, 02:40:00 PM »
Great, here we go again, people found another way to do stuff 'the easy way'.
I suggest also skipping the A/B at the end to save yourselves some hassle and an hour or two of time.
Does that remind anyone of the quick and dirty 15 minute rP/I2 meth synth? It sure does to me.

I'm not fat just horizontally disproportionate.

RoundBottom

  • Guest
no sarcasm needed.
« Reply #73 on: December 03, 2002, 02:53:00 PM »
i do not understand, is titration bad?  i'm just excited that it's higher yielding.  a rotovap is high on my list of TO GET. 

is it possible to remove the h2o from the titrated crystals?

...and i've never skipped an A/B... i've never done one  ;)

Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)

Osmium

  • Guest
More sarcasm
« Reply #74 on: December 03, 2002, 03:00:00 PM »
> i do not understand, is titration bad? 

Hell no, isn't it common knowledge that product quality decreases the more you work on purity?

> is it possible to remove the h2o from the titrated crystals?

Sure it is, but why would you? Yields would suffer!

> ...and i've never skipped an A/B... i've never done one

I know. Otherwise you would have ended up with much less toluene. But who wants quality anway, I'm sure you could even produce pills by drying and compressing the whole Al sludge with the freebase trapped inside.

I'm not fat just horizontally disproportionate.

hCiLdOdUeDn

  • Guest
HAHA funny sarcasm. SWIM trys to get as pure ...
« Reply #75 on: December 03, 2002, 03:09:00 PM »
HAHA funny sarcasm. SWIM trys to get as pure product but still maintain good yields. Distilling the freebase would be even better huh! ;)

Sink or SWIM

Rhodium

  • Guest
Acid/Base and Recrystallize!
« Reply #76 on: December 04, 2002, 02:37:00 AM »
Have you ever thought of the fact that the reason you get "less yield" when distilling your freebase and recrystallizing your final product is due to you removing impurities from your product, and that you will be left with only MDMA.HCl (which of course weighs less than MDMA.HCl + impurities)?