I wanted to pass on an observation about the new gakks and what may be a patient way of cleaning them out of the pseudo or the meth. I have noted that the metacrylates foul the crystallization process for both pseudo HCl and meth HCl. If you stubbornly continue to dissolve your product and recrystallize it again-- four times rather than two-- you see something I haven't seen before. The gakk starts letting loose and you can clean the amine.
After dissolving a gram of methacrylate gakked meth for the third time, on gentle heating, the alcohol/meth solution suddenly filled with a foggy, almost cloudy- but still almost fluid, very thin. This was filtered out and the alcohol reduced a little further. More of the same substance appeared; this also was filtered out. Acetone was added to the saturatured alcohol and good crystals grew in a short period of time. These crystals were rinsed and set aside, the mother liquor reduced down, a little acetone added, and chilled. The crystals that had been set aside were again dissolved in MeOH and heated gently. One more round of foggy stuff came out of the solution. Crystals formed readily as the solution cooled on the counter top.
This foggy gakk did not appear in the first crystallization, or the second, but did in the third and to a lesser extent on the fourth. The crystals burned clean on a foil test.
The remaining motherliquor was combined with alcohol washes of the beakers that had had pseudo in them; this solution was based, water added, tbe pseudo extracted into xylene which was gassed, yielding a good quantity of pseudo that burned completely clean on foil. No gakk.
A small reaction with this pseudo had no gakk, was of good quality, very clean, based easily, and crystallized readily. No gakk in it.
An earlier small reaction of some pseudo extracted in a less than successful experiment yielded meth that was belabored by the new gakk. The meth, on a third crystallization, started shedding the same foggy gakk in the alcohol; this filtered out easily, more formed and was filtered out. Crystal formation was greatly improved. More of the same stuff came out in the alcohol solution for the fourth crystallization. The meth from that formed crystals quickly and was relatively clean, and very effective. It was, unfortunately, a small quantity.
It seems that repeated recrystallizations breaks the stuff's grip on the amine. The gakk doesn't show (it can be smelled though) in the first two passes at making crystals. On the third or fourth pass, its starts coming loose.
Perserverence furthers. Perhaps. I may try to precipitate the salt form out into xylene or a naptha and xylene mix after having recrystallized it two or three times.
One other thing that seemed to work was basing the filtered alcohol solution. After filtering out the foggy gakk from an alcohol/pseudo mix that was the fourth time I had dissolved in alcohol, I added some water and NaOH to the alcohol; I extracted with xylene, washed it, dryed it, and gassed it... not expecting much. I was quite surprised, got much more than I expected, and the pseudo that I obtained burned clean on foil and reacted very well. No signs of gakk in the final product at all. It was as though the crystallization process got the gakk loose from the pseudo enough that basing the pseudo and gassing for the salt form again left the gakk behind.
I'm not suggesting this as a method of extraction, but hope the information might be useful.
