(Of Counsel)
08-25-03 14:27
No 455641
(Rated as: good read)
Recently SWIG tackled some Zyrtec D tablets for the second time. The first time he was innundated with orange nastiness that ate yield and made a mess. He extracted that time with the Straight to E procedure Video Editor posted.
He had never attempted to extract the pseudo from Allergan D tablets. My survey of information available here said they were tough to extract, and no one claimed particular success.
Procedure was a variant of Paying2Much's microwave solvent boils followed by VideoEditor's Straight to E. The Zyrtec pills were ground to fine powder and placed in a visionware glass sauce pan (with lid) in a microwave on high for a couple of minutes to dry completely. Xylene was added to the pan, covering the pill mass with about three cm of xylene. The mix was heated at full power in the microwave for five minutes, stirred, and returned to the microwave at full power. At about seven and a half minutes the xylene vapor was oozing out of the microwave, so the pan was removed, the pill mass stirred and allowed to settle, and the xylene decanted. The process was repeated with fresh xylene. After that the process was done twice with naptha, then twice with acetone. The lid allowed this to be done in the microwave, as the powder ws scraped off the interior of the lid and added to the pill mass before proceeding. After the acetone was decanted, the pill mass was placed in the microwave for three minutes of very low power to drive off the remaining acetone.
The pan was then filled with the STE's naptha/dried IPA alcohol mix and placed on the hot plate and brought to a rolling boil. The fluid was filtered off, the solids returned to the pan and the process repeated two more times. The filtered fluid was added to the amount of fresh xylene the Straight to E process suggests, and the mixture was brought to 105C, filtered, and the pseudo rinsed with acetone.
All solvents were collected in separate quart jars for comparison of what precipitated in each on cooling. On later examination the xylene contained cloudy precipitant and a little yellowish/brownish tint. The naptha had a layer at the bottom obviously more viscuous than naptha. The density was reminiscent of PEG. This had settled to the bottom. Another density layer appeared above this which was cloudy and off white; the rest of the naptha was in a less cloudy top layer. The acteone was slightly tinted brownish, and had abundant cellulose type precipitant. The naptha/xylene from the STE showed some coloration (yellowish) and some white precipitant, but very little solid matter compared to the solvents in the jars.
The same process was followed for extraction of the Allergan D capsules. These turned the xylene brown both times. There was a brown tint to the naptha after the boil, but it was much lighter than the xylene. The acetone had a very light brown tint to it. The alcohol/naptha solution was also light brown. The coloration remained in the naptha/xylene when the pseudo precipitated out. It was very white, very fine, and almost sandy in texture.
The batches were separately reduced in similar H3PO3/I2 reactions. The fluid from each reaction was washed with xylene and naptha, based with 20% NaOH solution, and the meth extracted into hot naptha which was titrated and the aqueous solution evaporated for the meth.
The zyrtech yielded two and half grams of meth powder from four and a half grams of pseudo. SWIG has yet to do the third pull or to collect the remnants from the acetone rinse or the alcohol wash of the evaporation dish. There was no orange anything anywhere this time, even though based with NaOH. The crystals formed in a MeOH/acetone solution, very slowly at first, then after what seemed to be a slow start formed decent crystals. A second crystallization produced expected crystal growth within the usual time span. These crystals smoke cleanly unless overheated, but leave a blackish ash when burned. They vaporize with little if any trace on foil or glass with gentle heating.
The Allergan tablets produced waxy brown cubic "crystals" in the xylene. These covered the bottom and sides of the jar three and in on the bottom four layers deep. The layers were about 1.5 cm in total thickness. I hesitate to call them crystals, but they were of uniform size, cubic form, and neatly distributed in even rows on the sides of the jar. The naptha jar contained a white precipitant that caked to the side of the jar and had to be scrubbed off by hand with an scouring pad. The acetone showed cellulose type precipitant on cooling. On cooling there was a cloudy, turbid layer that had a pale orange color. Six or seven small globs of orange, BB size at most, were at the bottom of the jar.
The meth from the Allergan-derived pseudo was quites strong and very smooth. It did have a contaminant which gave it a taste when smoked. The meth was dissolved in hot MeOH and filtered. The plug showed a fine grayish trace. The alcohol was reduced to saturation, and while reducing it a white precipitant formed in the alcohol. This was filtered out. Small whitish meth crystals formed in the MeOH/acetone mixture. These were filtered and rinsed, and weighed just over six grams. The solution was chilled without effect. It was then reheated and more cloudy/waxyish precipitant appeared and was filtered out. The solution then thickened over low heat and acetone was added and the solution allowed to cool overnight. In the morning no additional crystals had formed; some very small white particles the size of salt grains on table salt had formed, floating in the mixture. These did not resemble meth crystals and were filtered out. The color was slightly brown, the texture was waxy (or PEGish) and the white stuff melted into the filter. Crystals began growing in the solution then which was left alone to allow them to grow.crystals after this was removed from the mix. SWIG hopes the yield from this is at least another couple of grams.
While zyrtec and Allergan are both prescription medicines and too expensive to use for our purposes, they are known to be heavily gakked and difficult to extract cleanly. Combining Payin2Much's microwave solvent boils with VideoEditor's Straight to E extraction technique successfully cleaned the Zyrtech D of the ingredient that was such a problem to SWIG the last time. He said he thought the pseudo from the Allergan D should be precipitated once more in xylene, or crystalized in an alcohol/acetone solution to polish it completely clean. With that understanding, it appears the microwave solvent heating combined with the straight to E degakked both of these fairly dirty, gakky pills just fine. The trash in the solvents and in the naptha/xylene left from the extraction indicated neither did all of the cleaning, but in combination cleaned the pseudo very well.
SWIG things this combination of methods should have application to the OTC pills we use as a source of psuedo and will try it when he can get enough OTC white 60's, gakked or ungakked, to test. The method may work without further cleaning, but at the most a single pseudo precipitation in xylene or a dual solvent recrystalization should remove what little anti-crystalizing gakk was still present. That, he submits, is progress in the current effort to avoid the latest gakks.
The meth from both batches was very good, and from the second one was very smooth and much more potent that he realized at first. He did more than enough right out of the evaporation dish and wasted a lot of time being unable to stay focused. He wasted most of the rest of the day being pleasantly at odds with reason and good judgment, and unable to do anything one might consider "work" -- a fitting state of mind to be in on a Sunday afternoon, in his opinion.
Cookie Monster
(Hive Bee)
08-25-03 22:29
No 455716
He did more than enough right out of the evaporation dish and wasted a lot of time being unable to stay focused. He wasted most of the rest of the day being pleasantly at odds with reason and good judgment, and unable to do anything one might consider "work" -- a fitting state of mind to be in on a Sunday afternoon, in his opinion.
I know the feeling, how long did ya reflux? 36 hours?
I got one of those visionware saucepans but i never thought about using it with the lid on in the microwave. It does work much better in the microwave compared to a beaker. A beaker can get too hot really quick and burn the contents but i never had this happen with my visionware pan. Did you set it in the middle of the oven? My microwave has a turntable and i have found that putting the pan on the outer most edge of the turntable helpls to achieve a less bumpy boil. Ill have to try using the lid next time.
It wasn't Me!
(Of Counsel)
08-26-03 10:03
No 455803
Shorty: I ran the reaction for six hours as I recall. I had some extraneous considerations that dictated the shorter time. My microwave at the lab has a turntable and I place the sauce pan off center on the turntable. The lid really makes it possible to do the acetone boil in the microwave.
I was very close to clean pseudo with the method I employed. I will try this again and include on more final cleaning step when I do to see if the last of the orange will succumb to the microwave boils. Wouldn't it be nice to find that we were just cutting a corner we should not have been cutting, and knew how to avoid these ingredients' effect all along?
Cookie Monster
(Hive Bee)
08-26-03 19:18
No 455883
Experiment a little myself. I took 300 white 60's w/trip and put them in my visionware sauce pan straight out of the box (not ground up). I then covered with acetone and put my lid on the saucepan and place in microwave on high for about 3 minutes. I removed and the pills looked the same as when i first put them in. The acetone was slightly clouded but not much. I poured off the acetone and added some more new along with about twice that amount of methanol. Put the lid back on the pan and into the microwave.
This was boiled on high setting for another 3 minutes and upon checking the pills were still entact however each one was cracked open. There was no loose powder what so ever just a crack in every pill. So i poured off the liquid through a filter and added more acetone and methanol and repeated the process. Again there was still no free powder in the pan.
The filtered solution was then added to xylene and after psuedo was precipitated 2 twice and then washed with acetone the final yeild was 10.6g of very clean pseudo.
When the pills had dried out (which didn't take long) i weighed one to and it was .16g. The weight of these pills before extracting is .23g per pill. I weighed a few more and most weighed .15 -.18g each. Since one pill should have .06 grams of psuedo then i should have been left with .17g in each. I only did 2 pulls and i thing i should do a third which i plan to do the same way. Will report final yeild shortly.
It wasn't Me!