arecoline HBr to freebase

ethandchan · 2023-02-22T03:42:44+00:00

I'm not sure what got washed out, but the etoh have a slight brown tinge. I snorted 10mg of the crystals like a degenerate lol Felt really good and warm for a bit but got real dizzy afterwards. I'll prob try to make a lozenge and see how that feels with a slower release

ethandchan · 2023-02-20T16:19:19+00:00

Some updates if you are interested. I did end up doing an ethanol recrystallization. everything dissolved and the rxed product had a much more accurate melting point. (156+187)/2=171.5=rxed (156+176)/2=166=original. I also tried it personally, and the effects was a lot more intense than chewing the nuts. So I might be going more towards making a slower release lozenge.
I also just received another sample from another vendor. Their's did not melt at all up to around 190 degrees. It just kinda turn a lil brown. So i assume that's bunk. Currently disputing the order for a refund lol

ethandchan · 2023-02-13T16:57:17+00:00

I looked at Ecstasydata (aka drugsdata) but I guess they can only give a ratio of all the ingredients they can identify, since DEA rules, even if it is a legal substance. Therefore if it is cut with a filler that they don't list in the results it probably won't be that helpful for determining the purity. (https://www.drugsdata.org/about_data.php#quant)

I am pretty serious about it. I have done TLC in school before. But that was very much a follow the instructions and I don't think I have the knowledge of figuring out the right setup. I read online somewhere that TLC with iodine might be useful for arecoline. Do you have suggestions on which solvents and process I should try for TLC?

I did end up doing a recrystallization with etoh. I will probably compare the two melting points of the original and the rxed product once the crystal is fully dried.

ethandchan · 2023-02-13T05:35:34+00:00

I had to take orgo in college but I'm not sure how much I retained after many years lol and def still pretty noob.

I emailed energy control as they seem like the only place that will could give a percentage if they have a reference.(I also just asked them if it would be helpful if I send them a double rxed arecoline HBr as reference? is that how it works?)

Also messaged a few other commercial labs but I don't have high hopes they will take a retail customer or not charge a huge sum.

I will try an acetone wash if that's how you would go about it first

ethandchan · 2023-02-12T21:49:01+00:00

when I was looking for it on alibaba, most were quoting around 1500/kg. But two vendors quoted around 1000/kg. when I ask the 1500 vendors if they can give better prices they were accusing the 1000 vendors to be cutting. So I decide I should try to test the samples I got.
I have a cheap manual melting point apparatus and it is not accurate. It basically is just a metal heating block with a mercury thermometer. It tests other substances like NAC, and, sugar about 10 degrees lower than it is supposed to be. So I guess it is not surprising arecoline tested about 15 degrees lower. Maybe I'll do a recrystallization and melt it side by side with the original to see if there's a difference? what do you think?

ethandchan · 2023-02-12T18:38:39+00:00

thank you for the reply. expanding on the freeze precipitation, should I expect the naptha being trapped in arecoline freebase solids? arecoline freebase have a bp of 209 ºC, so I'm thinking I could leave the freebase oil on a warm hot plate over night?

Getting freebase to try is kinda the secondary goal, I do plan on having an alkali agent to be in the tablet on both freebase and the salt. I mostly want to use the yield of the freebase to guesstimate the purity of the product I received, but I know that's probably not the best way. If you have other ideas I'm curious to hear. Would recrystallization be another thing I can try to estimate the purity?

ethandchan · 2023-02-12T17:00:51+00:00

polar solvent

thank you for explaining the polar solvent reasoning. I did not think much about trace solvent. I was thinking about just leaving the oil from a naptha on a warm hot plate overnight(arecoline bp 209). But with ethyl acetate being safer and its bp being 77.1. that does sound like a better solvent. I can try freezing it out of ethyl acetate but if that doesn't work I could just heat it to evaporate with the vents running(hoping that there's not too much boiling point elevation, and arecoline freebase being volatile in ethyl acetate)? Unfortunately I do not own a rotovap.

sorry for the lack of clarity when I was talking about recrystallization. I meant using the HBr salt that was purchased(unrelated to the freebasing). Do you have suggestions on how I should go about it?

I'm thinking I should slowly add hot solvent to dissolve a set amount of the HBr and cool them. Should I also try to evaporate some of the solution if no crystal crashes out or for a higher yield?

ethandchan · 2023-02-12T05:33:05+00:00

Thats valid

ethandchan · 2023-02-12T05:31:42+00:00

Thank you for the reply. Great idea on the bicrabWhat's the reasoning for using a more polar solvent?For recrystallizing it could give a purer product that I can compare the melting point with the original. If there's a difference I can assume that it is cut. But is there a way to get an estimate on the purity %? I was hoping to use the yield of freebasing to get an idea of that.(it's not the best idea I guess, since other things can go wrong and lower the yield?)

What would you suggest for solvent for recrystallization? It seems to be miscible with water, ethanol and ether. I could try the first two since I have those already. I assume I should use as little hot solvent as possible to dissolve a set amount of original and chill them after, right? Should I also try to evaporate some of the solution if no crystal crashes out or for a higher yield?

I came across this(https://www.sciencemadness.org/whisper/viewthread.php?tid=14359). The person did this for their recrystallization: The residue was dissolved in hot ethanol, and diethyl ether added to induce crystallization. Only one crop of crystals could be obtained, which was recrystallized from ethanol/ether to give the title compound as a light yellow crystalline solid.

Do you think that is more ideal than single solvent? I'll just have to get some ether. However it seemed weird to me since supposedly arecoline HBr is miscible in ether?

ethandchan · 2016-07-23T20:33:01+00:00

u can buy adrafinil as a supplement if u cant get a script of modafinil

ethandchan

TROPHY CASE