Melting temps

[rangahtank]

Melting temps is all that SWIR has been going by.  Did the 'turn up the heat slowly 'til it just starts to melt' thing.  Kept the temp as constant as possible.  The crystals look amazing, just wanted to know if anyone has had any gaks still on the crystals?

[geezmeister]

I had one pass that produced yellow crystals. These were oily. Nasty. I scraped them all together and distilled them again, a little lower temp. These crystals were very white, no yellow, no oil. That made me realize that one wants a very stable heat source doing this. An oil bath or sand and oil should work fine if you bring the temp up slowly.

[Shane_Warne]

A thought crossed my mind that maybe pre-heating the GUP before doing the clean -> SPD, might help with the cleanliness.

'Ephedrine Hydrochloride. C10H15ON·HCl
Prismatic needles, mp 216°C., [á]D22 -32.5°. Easily soluble in alcohol and water. Its aqueous solation is stable at boiling temperature.

Ephedrine Sulfate. C10H15ON·H2SO4
Hexagonal plates; mp 257°C, [á]D22 -30°. Difficultly soluble in alcohol, easily soluble in water, neutral to litmus'

200C. I'd be inclined to try that with the correct license, I can just see some of those polymers dying in pain. Worth a try geez?

[geezmeister]

Your idea is to use dry heat on the GUPs, above the melting point of fb pseudo, to vaporize gakks that melt at or about that temperature, removing them so they won't be there when the fb pseudo is distilled. This might give you a wider temperature range to do the SPD without bringing gakks over with the vapors. Logical idea. The question may be whether the heating does more than melt a few gakks. That probably depends on what's in the particular pills.

One way to find out... try it!

You might consider heating just the extracted pseudo HCl rather than the GUPs. There are fewer substances in the mix at that point, but any gakk that would trouble the SPD will be there. If a gakk degrades at that temperature, solvent washes of the pseudo may remove the rest of that gakk before the pseudo is freebased.

Freebasing the pseudo may change the property of the gakk, too. The gakk's melting point may be different. The easiest way to find out is to try it and see what happens.

[Shane_Warne]

Thanks Geez.

Well with any luck it'll damage something.  
We'll see if anything in the GUP changes colour and/or condenses.

If there's a lot of condensate, a 2nd experiment can be done
to see what happens at different temperatures.
(hoping)


The question may be whether the heating does more than melt a few gakks. That probably depends on what's in the particular pills

Freebasing the pseudo may change the property of the gakk, too. The gakk's melting point may be different.

That's true. Well we'll know soon hopefully!

[rangahtank]

Well, to answer SWIR's own question:
Yes, some gaks do definitely carry over after the SPD and water rinses.
The process went as follows:
4 boxes generic 120's were ground up, then mixed with clear ammonia.  Just enough to make the 'marshmallow' result easily mixable, but not stiff. (Sorry, no ml measurement at the time).  Washing soda was then added IN SMALL INCREMENTS.  SWIR isn't sure why this makes a difference, but it does.  Adding it too fast, in large amounts doesn't allow the mixture to become liquid enough.  2X the pill mass volume of washing soda was added over time.

Xylene was added to this to equal 3X the volume of PM+Sodium Carbonate.  After thorough stirring, the mixture was allowed to settle and poured through a cotton ball filter.  This was done 3X.  Of the 9.6g theoretical total possible yield, SWIR got 7.1g for a total of 74% yield, a tad high.

The pfedHCL was then washed once with MEK, allowed to dry again, then a 25%NaOH solution was added to the pfed HCl to freebase.  This was filtered and rinsed with ice water 3X, then allowed to dry (THIS TAKES DAYS!).

The resulting dried pfed freebase was melted in a 500ml erlenmeyer flask with a test tube cold finger, half at a time.  The hotplate was turned up in small increments until melting was noted, allowed to sit at this temp for 30min, then cooled.  This was repeated 5 or 6 times.  The crystals that were dumped out and scraped off the test tube were AMAZING  Thin. Feathery. Perfect. 

All of the crystals were collected, then washed with ice cold distilled water again.  After drying, the crystals were dissolved in VM&P Naptha (hot) and the naptha was gassed to get the pfed HCl.

This was again rinsed with MEK, 2X.

After drying, the yield at this point was 4.2 g.  A much more realistic yield for SWIR at 44%.

This was reacted via the old LWR,  4.2gE, 3.4gMBRP and 5.1gI, and allowed to cook for 72 hours.  All regular reaction signs were noted.

  At the end of the cook, yellowish 'worms' of plastic looking gak were seen in the rp.  These were fished out, total weight of these were less than .2g. However, they were there, no further tests so gak was unknown.

Usual workup of post reaction, then gassing yielded 2.8g of methHCl.  Initial bioassay results were FanFUCKINGtabulous even before recrystallization.  Crystallization (SLOW) is ongoing.  Burn test was pure as the driven snow.

[Prepuce]

rangahtank, it sounds ilke you may have found the key that eluded SWIP for so long that he finally gave up on using ammonia for the primary extraction. Adding the washing soda a little at a time. Can it be? It would make sense. SWIP was doing just that in the early trials because he wasn't sure what the correct amount would be, but never worked his way up to 3x pill mass. He also used acetone vice MEK. Based on your results he's going to have to give it another try.

Why did it take so long for your fb to dry, though? SWIP uses ammonia sparingly, then when satisfied that everything is properly based, pours it out on a plate to dry in the air. It takes 3-4 hours with a fan blowing indirectly.

What you report sounds very much like the results he obtained with the method, especially in terms of final yeild. Initial reaction yeilds were not that high, and the final product had almost no remant of any gak. Just a slight yellow tinge to the post reaction solution that remained after washing with toluene, xylene, and once the solution was based, dH2O. The final yeild in clean product was about the same, and SWIP would describe the quality similarly.

PP

[rangahtank]

PP to answer your question:
Washing the fb with distilled water rather than some organic, fast drying solvent adds considerable drying time in this neck of the north woods.

Still unsure what those gak-worms were, but guess it's a moot point since everything worked.

Adding the washing soda slowly made a world of difference.  The mixture becomes much more liquid, therefore more washing soda can be added before it starts to form the hard, dryish clumps.

[BullwinkleMoose]

Xylene was added to this to equal 3X the volume of PM+Sodium Carbonate.  After thorough stirring, the mixture was allowed to settle and poured through a cotton ball filter.  This was done 3X.  Of the 9.6g theoretical total possible yield, SWIR got 7.1g for a total of 74% yield, a tad high.

The pfedHCL was then washed once with MEK, allowed to dry again, then a 25%NaOH solution was added to the pfed HCl to freebase.  This was filtered and rinsed with ice water 3X, then allowed to dry (THIS TAKES DAYS!).

is somthing missing here:  you go from having a non polar that has psseudo E dissolved in it ..... right into
washing a PseudoHcl with a NON polar  ...

did you gas or titrate and forget to mention it ?

[Prepuce]

rangahtank, you write:

"PP to answer your question:
Washing the fb with distilled water rather than some organic, fast drying solvent adds considerable drying time in this neck of the north woods."

Ammonium hydroxide is a fast drying solvent in your neck of the north woods? Must have something to do with the latitude.

PP

[Shane_Warne]

Water doesn't take long at all to dry. After 95% of it has been removed by filtration (regular filtration) stick it in the oven or beside a heater.

No solvent takes long in such a small residual amount, well not anything used for cleaning.

I won't have time to test that pre-heating shit btw or anything PI related.

[rangahtank]

Ooops, yep, a step was skipped in the initial write-up.  The pfed fb was GASSED after dissolving it in hot naptha. 

SWIR has read too many stories about losing some pfed due to overheating/quick drying, so after rinsing thoroughly with dH20 the filter and now based and rinsed pfed is allowed to dry slowly.  Yield loss always seems to occur for SWIR if he  gets antsy and goes too fast with the drying thing.

Second run and some different pills have yielded approximately the same results.  Seems to work swell PP, thanks for pointing SWIR in this direction.