My version of how NOT to cook

[SoldadoDeDrogas]

I've studied a little bit of organic chem on my own time in the past, atleast 10 years ago. I have been on this forum for about a month, and have thus been aiming towards a destination since. So, friends, here are my findings so far.
A SNB experiment was undertaken 2 weeks ago, that yielded a about a gram and a half of some kind of waxy, slighly psychoactive residue that was water soluable via water titration. For a first attempt, I'll call that a push. Not sure it is was under or over reacted. I can give details if anyone wants to know more about this. I'd love to know more, but this isn't the means by which I want to get to my destination in the future.
Very recently a rp/i experiment was undertaken. Note: A recipe or set of instructions is not stumbled upon and blindly executed without much forethought. If an experiment is the subject of an undertaking, it faces wide scrutiny. After hearing enough stories about people burying their tubs full of charcoal and gun bluing and yielding kilo upon kilo, it becomes essential to understand the mechanisms that are taking place to arrive at the desired destination.
To sum up, someone here I believe said it very, very well, something like - "don't just read a tek and try to execute it. Study a method or "route", study enough different variations of this route to understand whats important and necessary and why, and what is the variation, and then you can begin to understand and innovate from there." Having said that, my attempts of said method are usually a combination of various teks of the general procedure, the common themes that seem to work or make sense. Not sure if this is the best approach for a noobie on their own, as it leaves wide window for variables as opposed to following a tek to the tee and deciding yay or nay.

For example, the rp/i route, includes teks where a "push/pull" system of connected vessels is utilized, (I guess the pressurization or purity of reaction greatly speeds the process). Another version is the red-p cook 101 video, where the gentleman adds the water, rp and i and then waits a little before adding the PSE, proceeding to cook it for about 90 minutes, before continuing. Yet another version claims that everything must be added to the RV and refluxed for 24 hours. 12 hours converting %50, 18 hours converting %75 etc. The full 24 of reflux gives the total conversion. So, for the inexperienced, it's somewhat difficult to discern fact and fiction with such a wide window to aim for.

I'm all for less time in the field with my pants down, so I opted for the push pull, as it was supposed to be the fastest conversion for this route. As of the moment, I'm trying to make do with whats available at my disposal. My solutions to lack of tech, equipment, money, etc are somewhat primitive, ghetto, etc. Though they may work or be effective, this is something that shouldn't be taken lightly. You are doing this at your own risk of safety and freedom, and expense, as well as that of others, seriously! Use the proper shit!

And so, having studied various methods of a rp/i experiments, Taken from Festers SOMM 8th edition, "Ready Eddies recipie for push/pull rp/i" was decided upon and carried out. Ingredients are: 2grams of cleaned PSE from SU-24 (9*240mg), 1.2 of RP from around 100 strikers, and about 3 grams of I crystals sourced from %2 Iodine tincture. A few drops of water were added to help kick off reaction. After about 30 minutes of initiating the reaction, everything was going according to plan until catastrophic failure of RV, this is completely my fault as I was rushing, and being rushed, and not thinking that a ball mason jar might fail on me with enough applied heat. So the bottom fell out of my RV and I lost maybe a quarter to half of my reaction contents on the floor. I was able to use about 40ml of water to salvage and combine what I could into a pyrex cup. The method states that if the reaction doesn't go as desired, one can cook at 200F to finish the reaction and this is what was done. After cooking, everything loosened up, the dark color gave way to a lighter orange color, and the rp was quite visible and everything was unreactive with applied heat - this was the sign I was looking for. From here we cooled and filtered out the rp, adding about another 30ml of water. The orange color gave way to a more golden color. A roughly %20 NaOH solution was added to the reaction mixture slowly over the next 20 minutes. A pale yellow color was reached and small specks of oil were seen on top. Just a little more NaOH solution was added to be sure, and a slight film was noticed on top of the reaction mixture. The base was collected with 3*20ml toluene. The resulting 70ml or so of solvent was then gassed momentarily, until mixture became very cloudy. Some precipitate was noticed. Another moment or two of gassing to be on the "safe side" ended up turning the solvent into biphase. A Brown slightly reddish looking oil was pushed to the bottom of the solvent after the last little exposure to the HCl gas. This was not expected. A gravity filter was used and was turned away from for just a moment only to realize everything was back in solution and my filter paper with a hole eaten though and black residue all around as if burned. Filtration was attempted again and watched. The solvent passes through no problem, when the brown/red part (which smells somewhat fishy) passes though last, it starts eating away at the filter paper, turning it black and ruining the attempt. What was left of the solution after trying to filter, was then placed to the side and accidently combined with the remainer of %20 NaOH solution in H2O where it lost its color and turned very light yellow again as it was during basing.

This information should be received as a learning experience for some things that one should generally avoid. One of the main ones being, don't use a RV that isn't going to stand up to heat! No matter what the recipe says. Be safe, be careful, be prepared, stay calm and take your time, anticipate things going wrong and expect them to, because they will, so be ready!

Having said that, is there anything anyone can tell me about what the hell happened and if there is anything I can do to save what might be left of my product. I can give some better details about everything and have some pictures if needed. Also if you can please help me understand the finer points of a rp/i push pull reaction versus refluxing for 24h or just cooking it on the stove for 2 hours and then filter/base/gas. Thank you gentlemen in advance. Stay safe. o7

 

[SoldadoDeDrogas]

Here are some thoughts and observations in retrospect: With the push pull method, It is true, that the equalized pressure greatly reduces the time needed for the conversion, or 'cook'. Refluxing for 24h is the maximum time to make sure everything has been converted and no product is lost to evaporation. Red-P cook 101 demo says about an 90min on the stove after PSE has been added, reflux isn't mentioned. Fester says about 12 hours of light boil after adding PSE to hydriodic acid, recommends refluxing, or atleast rigging up a condensor with some copper tube around a long neck flask and cycling cold water. Another source specifies refluxing for 24h to fully cook. 18h = %75, 12h = %50 etc.

It is probably a good idea to react the RP and iodine first, without the E/PSE, and then filter out the RP so there can be a much cleaner reaction between the hydriodic acid and PSE.
Sodium thiosulfate is used as a "fail safe" to help protect against shoddy work, IE excess iodine and aziridine. It is not necessary, but helps the end product.
In the final step, when using HCl gas to precipitate, it is probably a good idea to filter through a dessicant, such as Mg2SO4, so there is no H2O and or other contanimation of product.
The smaller the batch is, the more susceptible it is to contaminants, skipping "optional" steps as listed above is done at the cost of your batch. Pretty sure my above experience is the result of atleast one of these consequences, if not a combination of all. I am pretty sure the oil I ended up with was ruined by excess iodine, water and alot of acid. As I said, probably wouldn't have been too noticible if I was making 100g, but only 1 or 2 g doesn't leave much room for error or carelessness.
In the future, much more time and care will be taken to ensure a higher level of production.

A small realization I made when dealing with gassing/pressurization of vessels is to make sure to use MALE when going out and FEMALE when taking in - I mean, that only makes sense right? It's not exactly obvious to a beginner - especially when one is improvising from scratch, it is not a subject I've ever seen mentioned when constructing a set up, or maybe I skipped class when it was taught. The bottom line of what I'm trying to say is to "go with the flow" as best possible - facing problems such as loose fittings or gaskets etc. will be minimized and possibility of bursting any seals will be reduced.

It seems there are different tiers of bb forum members. The haves, the have-nots, and the no fucking clues. Someone else said very well, "Any idiot can duplicate a reaction under perfect conditions in a laboratory environment so long as they paid their tuition." Alot of what everyone else is doing can be compared to art, a testament to the cook themself, as conditions, materials, ingredients, equipment, location etc. are all different. Getting something to work with another's set of instructions is really taken for granted for the miracle it is. Especially when you had to figure it out yourself, with trial and error, with most of the world leaning in on you and limited resources. A certain amount of luck is necessary, of course, but a new respect ought to be had for the high school drop out who can produce a very high grade product with optimal yields and efficiency with minimal waste, under extreme conditions and risk. To be able to do this with everything that came out of, say, Walmart, at ones discretion, I think, is a supernatural quality.