First time Birch SnB(modified) why fail (almost) + questions

[psyd]

Hi Hive! So finally I've attempted to make something myself - chosen the simplest available option - Birch in the bottle.
The output was unsatisfactory - from 3g of PSE pills got just ~100mg of product.
Here are the steps I've performed:
1. Extracted PSE from the pills (PSE + antihistamine) (one step extraction isopropanol+hexane+xylene). This step hardly is failure because I observed PSE crystals.
2. Skipped acetone wash (because instead of acetone I have unfortunately some nail cleaning liquid mixed with other solvents - it dissolves PSE Hcl too well).
3. Solved PSE in 50ml of water, added something like 10g of NaOH and 50ml of Xylene. Stirred for 15 minutes until no dissolved matter was in the beaker. Assumed that PSE has moved into freebase and solved in Xylene. Just in case, after removing top xylene layer, added hexane and stirred for 10 minutes then removed hexane layer.
4. In a 1L cola bottle reinforced the bottom by placing it into epoxy on outside and parafine inside. (Did that because previous attempt had 2 same bottles fail, with microruptures in the bottom). So i wanted to protect the fragile part.
5. Placed 50g baked MgSO4 in the bottle.
6. Placed 150g of finely ground NaOH into the bottle.
7. The powder left from extracting the pills placed in the bottle as well, thinking that in case something is left there, let it be put to use. Generally I thought it's better to have PSE already dissolved first, for easier reaction.
8. Placed xylene+hexane with PSE freebase in the bottle. Added 50ml more Xylene and 150ml more hexane.
9. Placed about 0.5g of Li into the bottle.
10. Placed 50g of NH4Cl into the bottle.
11. Since the reaction has not started, using silicone pipe and syringe added about 10ml of water with NaOH dissolved from beaker I used for PSE freebasing to the bottom of the bottle. No lithium was touched by water.
12. Light ammonia generation has started
13. Sealed the bottle, and covered the lid and top 2cm of the bottle with epoxy. (Previous attempt had bottle lid failure as well, so decided to reinforce the top as well)
14. The ammonia generation was happening slowly, I shaked the bottle few times, trying my best to avoid Li touching bottom layer. That increased generation speed.
15. The pressure needed to start forming bronze was reached after 1 hour of running. 2 hours later there was still mostly undissolved lithium and some tiny droplets of bronse.
16. Unfortunately I couldn't stay up anymore, I placed the bottle under a bucket in a safe place and decided to sleep a bit.
17. A bit turned into 6 hours. I checked the bottle, all Li was converted into bronse, floating atop the solvent Ammonia was still being generated, a tiny failure in the lid area was just venting ammonia out at very slow rate, without compromising pressure.
18. I assumed that after 6 hours the reaction should be done. Just in case I shaked the bottle, and left it for some more minutes. I assume there was no water, because bronze was not affected by shaking.
19. I puctured the bottle with a needle, let ammonia vent out, then cut the bottle open.
20. Top layer of solvent with bronze was moved into the beaker. Picture attached. I was so curious about the bronze (Li[NH3]4?), didn't want to discard it, so i took it with a spoon and moved to the mineral oil jar where i kept lithium.
21. Filtered everything, then washed the sediment in the bottle with another 100ml hexane+50ml Xylene and filtered.
22. Put solvent on a stirer and stirred without heating until no ammonia smell was present.
24. Left 10g baked MgSO4 in the solvent for 20 minutes, removed and filtered.
23. Gassed a lot of HCL through the solvent from h2so4+NaCl. (Maybe too much? The whole place was covered in HCL fumes, beaker smelled like HCL for like an hour after).
24. Tried to filter the solvent - got 0 powder on the filter.
25. There were some crystals and droplets on the bottom and walls (all about 100mg max), solved them with hot IPA, then moved to the dish for evaporating
26. Unfortunately what came out contained besides some small crystals some whitish oily mass, which tasted like the product as well.
27. Tasted more of it and indeed it works and it's expected substance, but 100mg is not what I expected from 3g of PSE.
So the questions:
1. Where is the product? If PSE didn't react, then it should have precipitated unreacted when gassing. This happened on a previous attempt when bottle has failed just when Li[NH3]4 started to form. Could it be that there's water in the solvent? What can I possibly do? Evaporate solvent? Is it okay to boil it?
2. Anything wrong with the reagents? Choice of solvents? I don't have diethyl ether unfortunately, and obtaining it might be risky here. Also I used NH4Cl, instead of NH4NO3 as recommended in all the guides, but I prefer Cl to NO3 in the vessel. Don't see why would it affect.
3. Was it running for too long? But bronze seem to be unconsumed, I'd expect bronze to be gone if the product would go subsequent reactions.
4. Li[NH3]4 seems to be such an interesing substance. What I've collected is still floating in mineral oil, only partially destroyed. Is there a solvent for it? Is it possible to prepare it separatedly, then add to unpressurized reaction vessel and expect PSE to undergo reduction? What possible solvent could solve and stabilize it in normal conditions? (I know liquid ammonia would do, but I imagine something without pressure/low temperature.) Maybe ionic liquid? What else can one do with it? I attempted this as my first synthesis because it's simple, but I'm curious of some less popular substances, can Li[NH3]4 be useful if I find a way to store it? Attaching the picture of how it looked in the beaker after moving from the bottle.

 

[SoldadoDeDrogas]

This one is a mess, my friend. I don't know where to begin to tell you where it went wrong.
For starters, 50g of baked Mg2SO4 is not necessary to add to the reaction.
The best advice I think I can give is to toss this and forget it and start over from scratch. Before you attempt to make something, spend some extra time to read and study and prepare for it. It helps to understand what you are doing and why you are doing it.
For example, where did you get the idea to add 50g baked epsom salts to the reaction? What did you think that was going to accomplish? The long and short of it is.. you didn't think. No blame. It is not until something goes terribly wrong that you will give this the respect it deserves, but sometimes your first big mistake is your last, when attempting things like this.

 

[psyd]

I followed the guide (pdf shared somewhere here) which suggested adding baked sodium carbonate to pull excessive water generated by NaOH/Ammonium salt reaction. Since I already had baked epsom salt, I used it instead. I guess judging by how slow the reaction was and that no lithium whatsoever was burned by water even after shaking this part worked.
I thought precisely for each step. Though maybe my conclusions were incorrect. Any other step seems I've done wrong you think?

 

[Raz]

I'm not even going to correct your errors. You should not be doing this. You put essentially a bomb under a bucket and went to bed.

 

[psyd]

Not really friendly With ammonia chloride it's at max just a cracker. I dunno why nitrate is recommended everywhere. And yeah bucket on stone floor with no flammables around would contain fire of 300ml of solvent for sure in case it happened. And yeah there was a person who didn't seep and with a fire extinguisher nearby.

 

[SoldadoDeDrogas]

I mean, I guess you got it to work... if you ended up with something to smoke at the end, and it was OK -
Now you just have to refine your work, .....alot.
You don't need epsom salts as part of the reaction because all that NaOH is going to soak up any water created. Any water that is created is immediately going to go towards helping the Ammonium and NaOH react anyway. Any excess water will be absorbed by NaOH, and won't effect freebase PSE noticibly anyway.
That initial 50g of epsom salts that was added to the reaction may have soaked up the freebase product? I'm not sure what happened to it all.
Quite possibly your mechanical technique is that fresh, and it is all sitting in the filter(s) or another error along the way in the process.
There may not be any point in extracting the PSE if you are going to add the mash right back to the reaction? Perhaps it gakked up and stuck to the sediment before it could be alkalined and extracted with solvent? I am just speculating here, of course.

Ammonuim nitrate is popular because it (was) readily available in instant cold packs at the pharmacy. Almost any ammonium salt will do (sulphate, phosphate, chloride etc.) I have only used nitrate myself. Xylene on its own will work OK for a solvent. I am not sure how the hexane effects the reaction but I don't think it hurts. If you can get coleman fuel or naptha thats probably your best bet. I would use Naphta with a spash of xylene, if you can. Virtually any non polar hydrocarbon will work. If you are using a store product, make sure to wash it if it contains any alcohol or acetone/MEK etc.

You can prep the fuel with ammonia/solved lithium before adding your EP/PSE. You just do the reaction without adding it. After your lithium has bronzed and dissolved, you can add the PSE and warm it a bit to help the process. It will take a few minutes (10?) for the PSE to freebase, then you can agitate the hell out of it to get the best reduction of PSE into meth - another 10-20 mins with PSE in prepped fuel.

Theres a few SnB teks up now, including one I wrote, each one varies but all of them are fundamentally sound. Read them all and try to understand what is necessary and what is optional and get a feel for the whole process all around. If you want you can message me and I can try to help more directly.

Good luck
o7

 

[psyd]

Thank you for the reply and advice! I think I figured out what happened - to use paraffin wax for bottle reinforcing was a mistake. I didn't think that it would actually work as a solvent, and it would move between liquid and solid phases when NaOH heats the bottle. My guess is that it has absorbed a lot of product. Also it has formed some liquid-gelly mixture with the solvents, making it extremely hard to evaporate completely and I had paraffin drops everywhere after drying (initially thought those are unformed crystals).
So I did following: I boiled everything, so paraffin dissolved, then I did AB extraction without gassing but in hot solvent/water. That helped to keep most of paraffin in the xylene/hexane mix. Added some toluene as well, to dissolve paraffin completely cause I'm out of xylene, but have a huge canister of toluene. Managed to get some more product, but still negligible, not even enough to grow crystals (well, anyway getting high on it for 2 days already, so I guess it paid the effort) .
That's great to know that I can use bronze without pressure! (Btw the bronze I collected 2 days ago, still is in the oil and half of it is still in bronze state! ) So I could do the reaction in some more pressure allowing vessel (a steel water tumbler maybe, won't steel affect bronze?) to produce bronze without risk of depressurizing and then reduce PSE in regular beaker!
Btw a question - is it okay to replace xylene completely with toluene? That's the only aromatic solvent I have left. I can't get coleman/naphta here, theese names are not even present in the market, cheapest option is Hexane. Also how to wash it from possible alcohol contamination? I prefer to order solvents not in specialized chemical shops, cause don't wan't to get on any watch lists. Otherwise I could just order ether, or even P/I for analysis. Many chem shops are willing to sell almost whatever, ether, mek, even 1,4 bdo, but who knows who's watching, (paranoia, paranoia, lol). But yeah, paint shops are not including certificate of analysis most of the time, they just swear that it's 100% pure. I already bought acetone which was sold as 100%, but then after it started dissolving what it shouldn't i managed to find the shop supplier and figured out that it's 85% acetone, rest 1-methoxy-propanol with 1-methoxy-2-propyl acetate according to what's on the supplier website.

 

[psyd]

Thank you for the reply and advice! I think I figured out what happened - to use paraffin wax for bottle reinforcing was a mistake. I didn't think that it would actually work as a solvent, and it would move between liquid and solid phases when NaOH heats the bottle. My guess is that it has absorbed a lot of product. Also it has formed some liquid-gelly mixture with the solvents, making it extremely hard to evaporate completely and I had paraffin drops everywhere after drying (initially thought those are unformed crystals).
So I did following: I boiled everything, so paraffin dissolved, then I did AB extraction without gassing but in hot solvent/water. That helped to keep most of paraffin in the xylene/hexane mix. Added some toluene as well, to dissolve paraffin completely cause I'm out of xylene, but have a huge canister of toluene. Managed to get some more product, but still negligible, not even enough to grow crystals (well, anyway getting high on it for 2 days already, so I guess it paid the effort) .
That's great to know that I can use bronze without pressure! (Btw the bronze I collected 2 days ago, still is in the oil and half of it is still in bronze state! ) So I could do the reaction in some more pressure allowing vessel (a steel water tumbler maybe, won't steel affect bronze?) to produce bronze without risk of depressurizing and then reduce PSE in regular beaker!
Btw a question - is it okay to replace xylene completely with toluene? That's the only aromatic solvent I have left. I can't get coleman/naphta here, theese names are not even present in the market, cheapest option is Hexane. Also how to wash it from possible alcohol contamination? I prefer to order solvents not in specialized chemical shops, cause don't wan't to get on any watch lists. Otherwise I could just order ether, or even P/I for analysis. Many chem shops are willing to sell almost whatever, ether, mek, even 1,4 bdo, but who knows who's watching, (paranoia, paranoia, lol). But yeah, paint shops are not including certificate of analysis most of the time, they just swear that it's 100% pure. I already bought acetone which was sold as 100%, but then after it started dissolving what it shouldn't i managed to find the shop supplier and figured out that it's 85% acetone, rest 1-methoxy-propanol with 1-methoxy-2-propyl acetate according to what's on the supplier website.

 

[SoldadoDeDrogas]

Yes you can use toluene instead of xylene. Virtually any non polar hydrocarbon will work. Midrange to aromatics will provide a more slower but steady reaction. You can wash them of alcohol and acetone by simply washing them with water a few times and seperating the phases, remember to dry with baked epsom salts or another dessicant at the end of the wash to eliminate any moisture.

Alot of these solvents and many others that can be substituted for our purposes can be found locally, you just have to know where to look and then put in the effort to wash and purify them, which just involves washing with water, distilling and drying with dessicant and you have lab grade solvents basically. Look in. Grocery stores, auto parts stores, hardware stores, walmart etc. You can do this reaction with SO MANY solvents it is ridiculous.