Waxy substances when extracting PSE free base (with pictures)

[calmcatfather]

Hello again friends. I tried to extract PSE free base using the "Universal Extraction Technique: Straight to Bee" method. I will write in detail here with pictures. At the end I get a waxy substance. Thanks in advance to those who have information on the subject.

First, let's start with the contents of the pills.

- ibuprofen
- pseudoephedrine hydrochloride
- ascorbic acid (Vitamin C)
- Calcium hydrogen phosphate anhydrous
- Croscarmellose sodium
- Povidone (k-30)
- Talk
- Microcrystalline cellulose (Type 101)
- Silicon dioxide-syloid 244
- Hydrogenated castor oil
- Hydroxypropylmethylcellulose E-15
- Polyvinyl alcohol
- Titanium dioxide
- Quinoline yellow aluminum lacquer
- lecithin
- Xanthan gum
- Sunset yellow aluminum lacquer

First, I made a subtraction by following the instructions exactly. The images after the subtraction are as follows.

Then, thinking that too much time had passed since I had tried this technique, I tried it again by changing it a little bit to my liking.

The things I changed for myself are using less acetone, less corn starch, and boiling it with petroleum ether before letting it dry too much.

Now I want to move on to my questions.
1- What exactly is the waxy substance in the first pictures?
2- If the waxy substance is correct, I then passed Toluene HCl gas to it, but I did not see any crystal pieces fall off or form. Did I pass too little HCl gas or did I need to pass more?
3- How long does it take for the free base to crystallize? Does it crystallize immediately or do I have to wait 12 hours etc.?
4- Can the free base be used in the RP/I2 reaction or do I need to convert it to the HCL salt?
5- For now, I have the pills whose contents I have written down. I would like to thank experienced and knowledgeable friends in advance if they share their experiences on how I can remove them.

 

[SoldadoDeDrogas]

Hello -
Not sure what the waxy substance is, assuming residue of the pills binder/blockers
If you are gassing and sure there is something that will precipitate, you keep gassing until no more precipitate is formed upon evolution of gas through fuel.
I don't know about crystallizing freebase.
The freebase can be used in a birch reaction (shake and bake method - ammonia and lithium). For RP/I2 is must be in acid salt form. HCl, sulfate, phosphate etc.
There is alot of information about cleaning the pills on this site, I have added a bit from my own experience. A menthanol or IPA extraction is usually all that is needed to isolate the EP/PSE from the pills and rest of the gak. Depending on the quanitity of EP/PSE, I would use more and other methods that will leave a better product. As far as a quick box or two of sudo, an alcohol pull is usually sufficient enough for a reduction.

 

[iceberg]

Hello master, if you (you) tried the shake and cook method and were successful, can you help me with this? I have never tried it and I want to learn from someone who has succeeded before. (People who have never tried it before copy and paste the forms) There is information pollution. Thank you.

 

[calmcatfather]

I'm not sure if there's anything that will precipitate. So I don't know much about how much I should gas it. From what I've researched, it says I should gas it to around Ph4-5. Does the free base crystallize or does it have a waxy appearance? I'm attaching a picture of a dried version of the free base I made this afternoon.

Methanol is a chemical that I can hardly find, but IPA or ethanol is a much more accessible alcohol for me. You said that there are easier methods in the forum. I looked through almost all of the topics in the forum and I couldn't understand exactly what you were talking about.

 

[SoldadoDeDrogas]

Yeah, I don't know about 'easier' methods. I said there was alot more information about cleaning pills all over this site. %91 IPA that you can distill or atleast dry with epsom salts should work fine, though if you could distill, methanol wouldn't be hard to come by. Whatever the alcohol is, it can't have any water, otherwise you are going to activate the things you are trying to get rid of. I don't know if they bind to the amine or how it works, but somehow the end product usually doesn't have good results.

The thing with HCl gassing is that you can't over do it. When it is done precipitating salt, then it is done, as there is no more product left to precipitate. So, basically, gas until it stops making snow.
To be clear, you are gassing the freebase meth (or ephedrine/pseudo) in hydrocarbon solution, or in other words, your meth or ephedra base oil is mixed into your solvent - naptha, ether, toluene etc.
When you introduce HCl gas you are precipitating the base oil into an acid salt when it becomes acidic and saturated. The acid salt does not dissolve in the fuel, so you filter. You should wash with cold, dry acetone to make sure impurities are removed - this step is more important for post reaction meth rather then ephedrine from pills. It doesn't really hurt if you choose to clean pills as long as you do it right and don't lose any (or significant) product. After the acetone rinse, you can recrystallze to make it look like ice, or you can let it dry and use it as is.

In your picture, I am guessing that is precipitated ephedrine/pseudo ? The freebase doesn't crystallize, it was freebase - you gassed it and turned it into HCl salt. -- Assuming that is what you did.
If that is the case, then when it dries, you should be able to proceed to reduction. Otherwise, I don't know. I don't know if you cleaned them right, how you did it, if you removed the ibuprofen .. or what?
I'm not sure how to test your EP/PSE to make sure you know if it is good to react ...

 

[calmcatfather]

- I have 99% IPA. And also ethanol. Just in case, if we dehydrate the ethanol with sodium sulfate and then soak the pills in ethanol instead of methanol, would we get the same effect?

The method I derived this from is the "Universal Extraction Technique: Straight to Bee" technique found on erowid.

- Next time I will measure the pH for gassing and do the crystals start to form right after gassing or do they start to come out slowly after gassing for a while?

- These are the final images of the free base, it has a slightly waxy shape. And 300mg of this substance came out of about 900mg. Can we assume with complete certainty that this is free base?

 

[SoldadoDeDrogas]

I would dehydrate and use the IPA, but they are all more or less interchangable for extracting pills.
"Straight to Bee" or straight to base, refers to the first(?) step - when you add your NaOH solution to the pills, the amine(s) come out as an oil (think cocaine into crack).
The idea is that you are leaving everything behind that you cannot extract with a hydrocarbon pull (naptha, ether, toluene etc.) Then when you gas, you are leaving everything behind that doesn't precipitate.

Measuring pH for gassing is generally unnecessary unless the instructions call for it. When gassing, it does not begin to precipitate immediately, after a minute or two it will look like poofs of smoke coming out of your gas tube - snowglobe. I am pretty sure you can't over do it, so when you don't see any more precip falling out, you're done.

If this is what came out after you gassed then it is not freebase. It is hydrochloride salt - freebase is the oil form. If that is your salt, it does not look like how pseudo HCl should look, it sounds like there is probably alot of ibuprofen. Dissolve everything in cold water and throw it in the freezer, cold water extraction to seperate the pseudo and ibuprofen. 30 minutes in the freezer and the pseudo will be dissolved in the water and all the ibuprofen will collect at the bottom as solids. Now you can filter it off, rinse it and evaporate and you should be left with crystalline pseudo HCl all by itself.

This whole straight to base thing is potentially an extra and unnecessary step in this whole process. With these pills, in the future, I believe you can just extract with a few anhydrous IPA pulls, filter and evaporate. You'll be left with pseudo and ibuprofen. Follow the IPA extraction by a simple cold water extraction on whatever is left after the IPA is evaporated as described above to seperate the pseudo and ibu. Let that dry, collect your pseudo, and you should be good to go...

 

[calmcatfather]

- In my next attempt, I will dry the IPA or Ethanol I have with sodium sulfate. As far as I understand, I will leave the powdered pills in it for a few hours with the anhydrous IPA. Then, after evaporating the IPA, I will add toluene and gassing it. (Will I do basification as a step in between?)

- I completely understand the gassing and precipitation process. If the extraction is correct and the free base PSE is in toluene, without checking the pH, the PSE hydrochloride salt will start to form and precipitate within a few minutes when gassing is done.

- What you see in these photos is what I extracted from the free base extraction procedure without any gassing. It is a waxy, oily substance. From what you described, I think this is the PSE free base. After gathering all the free bases together, I will add toluene and then gasify.

- One thing I don't understand is cold water extraction. Does PSE dissolve in normal temperature water and not in cold water? Is the idea behind it the dissolution temperature? In fact, the free base in this photo is not the hydrochloride salt. You said that PSE HCL will dissolve in water. The remaining ibuprofen will settle to the bottom as a solid. When I add water to this free base, the free base will not dissolve in water. If there is ibuprofen, how will I separate it from each other by extraction?

- My main goal is to directly form the hydrochloride salt. Since the hydrochloride salt did not form with a few methods I tried, my aim is to first extract the free base form and then gas it in toluene to form the salt.

- After a few shots of anhydrous IPA, the hydrochloride salt will dissolve in the water and if it remains, the ibuprofen will remain as a solid at the bottom. When I filter this and evaporate the water, does the hydrochloride salt form at the bottom or does it evaporate with the water. Because in almost all procedures that try to extract the hydrochloride salt, there are information and warnings about using water. When I add toluene to the PSE that passes into the water phase, the PSE passes the toluene? If the toluene is gasified later or left to evaporate, I will be successful?

- Thank you again for your comments, really valuable information and experiences.

 

[iceberg]

You should reduce the pH to 3 with the distilled water you use as a solvent, then I increased it to p13 with Naoh solution and added dmc and separated it. dmc is ph5-6 again, then I dried the water in it and evaporated it (it is said that toulene is more effective instead of dmc but I haven't tried it yet) I tried it with dcm and it was successful

 

[calmcatfather]

A new method was tried the other day. A box of pills was turned into powder. And about twice as much ethanol was added. It was left to rest for 12 hours and filtered. A crystal-like structure formed inside, but when this was checked with a glass stick, it started to disperse in the ethanol like a powder. But the cat noticed something. She saw crystals starting to form on the sides of the glass container where the solvent was. She took a finger-sized amount of the crystals and put them in her mouth and tasted them. The taste was really bitter. The bitterness didn't leave her tongue for a while. I think the cat thinks she's on the right track this time. Now she's thinking of putting it in a large pyrex container or something and slowly evaporating it. I guess when the ethanol remains as a bulk liquid, it doesn't crystallize.

 

[NAGAINAGAYOSHI]

Evee heard about chen kao test?

 

[calmcatfather]

Yes, I did some research after you mentioned it. A simple test to determine the presence of ephedrine, pseudoephedrine, etc. using acetic acid, copper(II) sulfate and sodium hydroxide. I really liked it. A simple test or reaction that is used to determine the presence of ephedrine or its derivatives in a very fast and simple way. I won't be able to try it right now because I don't have copper(II) sulfate. But it is thought that the crystalline material that accumulated and changed on the edges of the glass is pseudoephedrine because when anhydrous acetone was poured, the crystals started to clear up even more. Also, it does not dissolve in acetone.