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Hydriodic Acid - Phosphorous Acid Reduction

Novel Methamphetamine Synthesis from Pseudoephedrine

by Geezmeister

A short time ago SWIG poured ten ml of dH20 into a flask and added 10.5 grams of phosphorous acid flakes. These were swirled until the acid mostly dissolved, leaving a few flakes still to be dissolved. This was not particularly exothermic. To this mixture was added 11.5 grams of very dry I2 obtained from tincture which had been fairly well powdered before adding; this was stirred until it appeared to have dissolved and the mass resembled a mixture of dark crude oil. Ten grams of pseudoephedrine freebase crystals were added to the solution and stirred until they appeared to have dissolved or dispersed uniformly throughout the mixture.

The flask was placed in an oil bath and a 400 mm Liebig condenser fitted. Water with a temperature a little above freezing was circulated and the oil was slowly heated. A thermometer suspended into the flask through the condenser was used to monitor the temperature of the flask contents.

When the contents of the flask reached 80° a reaction began which produced a thick yellowish smoke for a few seconds; this quickly gave way to white smoke, not as dense, which cleared to a thin white smoke, became a mere wisp, then dissapeared entirely. A balloon was quickly fitted to the condenser when gas production began; it filled to softball size and remained there until it was necessary to remove it to lower the thermometer. No noticeable gas loss occured during the reaction. This reaction took place very quickly and violently, and did not last very long. It was similar to the reaction which occurs when I2 is added to hypophosphorous acid. It was as vigorous, as quick, and as short lived as that observed with hypo.

The contents of the flask went from dark black to thick, creamy pale yellow. The contents of the flask began to bubble steadily, although not with the vigor or number of bubbles observed with a hypo cook.

As the temperature inside the flask reached 90° the color of the solution darkened. Bubbling remained the same. At 100°C the mixture was even-textured and resembled vanilla pudding. At 107° the contents of the flask became noticeably more active and the mixture was clearing and becoming transparent. SWIG's best estimate of the time elapsed to this point is about twenty five minutes.

When the mixture reached 110° its color appeared to change to gold, but this may be affected by the color of the oil bath. It also became completely transparent. Clear. You could see the bottom of the container holding the oil clearly. No solids were in the flask. Again, this reminded SWIG of a hypophosphorous/I2 reaction after the bubbling in the latter becomes hard to sustain without continuous heat, and the reaction nears completion.

My intention was to bring the internal temperature of the flask to 118° and reflux for the night. The oil bath reached a maximum temperature of 170° (measured by a candy thermometer) I was unable to get an accuate reading of the thermometer in the flask because of the heavy condensation on the walls of the condenser and the failure of SWIG's knot in the string suspending the thermometer. (Okay, SWIG was not a good boy scout.)

At approximately 1:00 am SWIG concluded that the oil bath temperature at its maximum setting would not heat the bath beyond 170°C, the flask's internal temperature waould not get hotter than 112-114°C, and the reflux would remain stable about half way up the condenser unless the water in the reservoir got too warm over time. SWIG decided he might as well leave the reaction as it was. The reservoir of water was replaced with fresh cold water. No difficultly had been encountered with the heat produced by the reaction at that time.

The mixture will be allowed to reflux for approximately eighteen hours, at which time SWIG will be free from the chains of employers and other obligations and be free to pursue his avocation as an alchemist.

The reaction is being monitored by his ill humored assistant and sidekick, who was given bread and beer before being chained to the water pipes in the lab and told not to fall asleep until SWIG returned.

SWIG observed that the reaction proceeds much the same way that a hypo reaction does, at least after it reaches the intial 80° temperature--which seemed to be the temperature at which the phosphorus acid and I2 reacted and made HI. From that point the reaction proceeded as fast as a hypo reaction does to a clear state. The color of the mixture could not be determined while the flask was in the oil bath; the color of the oil and transparency of the mixture made judging the color difficult. The time between first heating and becoming transparent was a sufficient period for a hypo reaction to have completed.

SWIG has discussed the reaction with a couple of street cooks in his area. They told him they had been taught to dissolve the phosphorous acid in water, add the ephedrine, then add the I2, and put it on heat with a sturdy balloon until it really goes wild. They are instructed that when the contents of the flask become clear, as long as it has been fifteen minutes, the cook should be considered as complete. SWIG believes they are quitting too soon. He thinkgs their mixture is being pulled to quickly and has not completed at this point. His bioassays of the product of other cooks' phos acid meth leave him with the impression of half-reacted, unfinished meth, not unlike what is obtained after a short, hot, dry cook with very clean pseudo and fresh red phos. Good for street dope, not complete by SWIG's standards.

SWIG is concerned about not being able to achieve the intended 118° temp inside the flask with the oil bath. He otherwise has the feeling that the synth is similar to the hypo synth and that if the inital concentration of HI is high enough it should complete fairly quickly and completely. All the same, he wanted to reflux the mixture to give it every opportunity to finish.



SWIG got to the lab about seven last night. He sniffed the top of the condenser and smelled that smell he loves to smell. He turned off the oil bath, removed the condenser, and took the flask out of the bath so he could get a good look at it. Pure gold. Reminded him of the look of the flask after a hypo/I2 cook completes. The honey was, however, a good deal more viscuous than the honey from a hypo cook.

He added boiling dH20, three times the volume of the honey, to the flask and swirled until the honey was thinned out. There is nothing to filter out of the honey. The honey is thick and oily, and if filtered a lot of it would be trapped by the filter. The honey is washed with xylene, then hot naptha. Neither solvent appears to be contaminated with reaction byproducts. The honey is based with a 20% NaOH solution. It bases very quickly with less NaOH than is usually necessary after a rp/I2 cook.

Hot naptha is added to the flask and the contents swirled several times. The naptha is allowed to sit on the honey for ten minutes, then is decanted. This process is repeated and the two volumes of naptha combined and washed with brine, then warm water, then cool water. The rinse water is added to the based honey in a coffee pot and a third volume of naptha added. A little additional base is added to the honey, which is then heated slowly until it just begins to boil. The coffee pot with honey is removed from the heat, covered, and put away for processing in a day or two.

The meth was extracted with dilute aqueous HCl. The evaporation dish skinned completely over. The meth was almost transparent even in this state. The contents of the dish were flashed with acetone which mostly boiled off, leaving a good quantity of very white crystals. A sample was set aside for testing, the meth panned to one corner, and acetone collected and placed in the freezer. The meth was rinsed once with fresh acetone, which was also collected for later use. Boiling IPA was added to the evaporation dish to dissolve the methamphetamine. The alcohol solution was filtered through a Charmin Plug, concentrated to near saturation, and acetone added. The beaker containing the solution was left on the counter in a room with an ambient temperature of about 50 degrees F.

While practically all the material panned to the corner of the evaporation dish dissolved readily in hot IPA, the Charmin plug collected a noticeable small layer of slightly pinkish fine clay-like particles. These particles had a smell similar to the odor one sometimes found in meth produced with an excess of hypo.

The test sample from the evaporation dish was placed on foil and melted. It gave off an odor found where an excess of hypo was used in the reaction. The vapor had a bitter, nasty taste. Very light brown to tan deposits remained on the foil after the sample was vaporized.

After two hours the crystals which had precipitated in the alcohol solution were filtered off. The mother liquor was filtered through a Charmin plug, this one more packed more tightly than the previous one. This filtering also left a small layer of very fine dark pinkish tinted clay-like powder on the plug. The motherliquor was concentrated and the beaker placed in the refrigerator. In about an hour the crystals which had formed were harvested and the motherliquor combined with the alcohol used to rinse the evaporation dish, the funnels, and glassware that might contain meth. The filters used to harvest the crystals were soaked in alcohol, wrung out, and that alcohol added to the beaker. This was again filtered and concentrated, covered, and placed on a shelf in the cool room for crystal formation and later collection.

The collected crystals weighed 4.7 grams. This does not represent the yield from the first two pulls as there is still a significant amount of meth in the alcohol solution which should form crystals. The third pull should add to the overall yield.

The crystalized product, when vaporized, did not have the smell noted earlier nor did it have any unpleasant or noticeable taste. This must be contained in the fine silt that Charmin plug removed. The vapor is very smooth to inhale. SWIG inhaled about five or six good pulls from a pipe before realizing he should have quit after four. this does not seem to have the same strength as the product of a long wet rP/I2 reflux, but it is very close. With refinement of the synth and some experimentation with the temperature and perhaps a little less phosphorous acid or a little bit more I2 the results should be equivalent to the product of a hypophosphorous/I2 reaction.

Initial impression was that this synth definitely does work as advertised. Dual Friedrich condensers are sheer overkill. Cold water will be sufficient if one uses a 400 mm or longer condenser. Heat was not a problem after all. Gas containment was not a problem.

The violent reaction described in the writeup is the same HI producing reaction one encounters adding I2 to hypophosphorous acid. The reaction takes place immediately with hypo. With phosphorous acid, it did not take place until the solution reached approximately 80°C. At that time it proceeded with a vigor similar to that of the hypo/I2 reaction forming HI, and just as fast. No significant bubbling occurred until the temperature of the solution was at or above 100°C. The bubbles were never that small, and this is attributed to the viscosity of the solution. SWIG did not have a stirrer, and believes that a stirrer would be a a good addition. The solution is not as fluid as a hypo solution or a redP/I2 solution and is too thick to allow bubbling of the type SWIG tries to achieve in the other reactions. The viscosity may make complete reduction a little harder to obtain without stirring.

SWIG is of the opinion that a reflux at 118° is not necessary. He did manage to measure the internal flask temperature and it reached 114°. The deep fat fryer he used will not reach its stated maximum temperature, but it does come close. SWIG thinks the higher temp is not necessary. He plans to run the next such reaction in the 100-105° range. The reaction may complete quite satisfactorily at or above 80°. SWIG thinks the author of the writeup selected the boiling point of the solution as the reaction temperature and that the selection was not made for reasons relating to the reduction of ephedrine.

After arriving at home SWIG did note a slight twinge of paranoia associated with the meth, although nothing along the lines of shadow people or faces in the woods. He thinks the higher temp may be responsible for this. On the other hand, he does not notice any jaw tightness or teeth grinding, and he ususally detects the start of that problem if the cooking temperature exceeds 107-110.

The synth itself is quite easy. It has several good aspects worth noting, aside from the availability of the phosphorous acid. Not needing to filter the contents of the flask allows washing and basing of the honey in the flask. Given the right flask, no separatory funnel would be needed to extract the meth. The volumetric flask SWIG used allowed him to neatly decant the solvent without difficulty. Yield should be in the excellent range. The product is almost as potent as the product of his recent long refluxes, and he beieves a little adjustment in technique, temperature and equipment will achieve the same potentcy as the hypo cook does. Yield may be in the same range as the hypo cook, and if it is this synth may be the synth of choice for the clandestine cook.

Over all the synth reminds him a great deal of the hypophosphorous synth, only this synth is safer and does not have shelf life concerns and concentration concerns that the hypo synth entails.

His current impression is to buy stock in companies that manufacture phosphorous acid, although he may just buy the acid itself until it is listed, which is inevitable and may happen fairly soon, as this synth is becoming more widespread and may catch on like wildfire.

Imagine. No more matchbook strikers to scrape.

The reaction used pseudoephedrine freebase derived from 120 time release caplets. The pseudo was very clean, extracted by the Straight to Bee method subsequent to xylene, naptha, and acetone boils. SWIG has no idea how pseudo that is not this clean would react.

Conclusion is that the synth does in fact work, works well, and may replace I2/redP as the standard HI synth.

Do not be afraid to do this synth. It works.



SWIG did not close an eye last night and has been hard at it at work since he posted this a.m. about the results of the synth. He notes that his last puff was about seven this morning while getting ready to leave for work. He does not need another puff at this time, is doing just fine, feels good, and notes today only side effects aside from productivity (without tweaking around) is that his attention has been distracted repeatedly all day by most female forms he has had cross his field of vision. Okay. so that happens every day too. He just noticed it more today.

The stuff is smooth as glass and has a very pleasant effect. I note my jaw muscles are tight which suggests I have been gritting my teeth. I suspect dropping the temperature to the 100°C range will avoid that problem on the next batch. At lunch a friend of mine was treated to a nice little three puff line on heavy foil. I noted the little diamonds I gave her melted cleanly, rocked right up, and when they were gone the foil was still clean. When I left to return to work, she had a smile on her face and an attitude that suggested she would be busy all afternoon.

I am anxious to check my solution in the beakers to see what diamonds may be lurking in the solution, but may wait until tomorrow to do so, since I have more than enough for a few days as it is in the half gram sack I stashed at home.

I am impressed with the synth and note that it reacts like the concentrated hypophosphorous acid/ I2 synth. No doubt the reflux allowed for complete reduction, but it is very likely that a shorter reflux would suffice. This synth definitely merits further study. coolcoolcool Any synth that gives you product you don't think about going back and getting "just a little more" anytime soon after first do it is worth checking out.

Thanks to Rhodium for bringing this to our attention. I just wished I'd done the synth a little earlier.