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HCl/HBr salt test

Anon0631

Anon0631

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Is there any way to differentiate 2c-b HCl from 2c-b HBr?

Presumably if i possessed samples of both, I could look at which one was less soluble in water. But let's say I had just one sample as an unknown salt?
 
^ is there a way to predict how much of a NaOH solution at a certain concentration it will take to neutralise x mg of each salt?

Coming back to solubility, it appears from some reading around that there really is a drastic difference between the two salts. 2c-b HCl will dissolve at about 5mg/ml whereas 2c-b HBr will dissolve at approximately 10 times that concentration.

So... If I can dissolve 20mg in 1ml of distilled H2O at room temperature. It's the HBr salt.

Does this sound about right?
 
I think that unless you can be sure of the purity, you cannot properly draw conclusions on the results of such experiments. But yes I think if those numbers are not only estimates, the difference in solubility could be more significant than the purity margins. However be sure to keep your conditions consistent with the conditions at which the solubilities were measured. It would be a shame to use tap water at some happenstance temperature, though maybe that is not even significant - still don't take that chance.
 
Well, yes, actually, but only if you have a significant quantity of the salt. NaBr is soluble in dry ethanol, whereas NaCl is not, so adding some NaBr to dry ethanol followed by the unknown form of 2C-B will create a precipitate if you have the hydrochloride, but not if you have the hydrobromide. Unfortunately this test requires ethanol with very little water content, I doubt everclear would work.

Refs:

http://en.wikipedia.org/wiki/Sodium_chloride
http://www.scribd.com/doc/30127869/Sodium-Halides

"One gram of sodium bromide dissolves in about 16mL of ethanol" compared to roughly 2 L of ethanol to dissolve a gram of NaCl.

Why, though, do you need to differentiate between the salts?
 
Nope. It's pertinent to wanting the HCl consistently from purchase to purchase so I can rely on dosing being the same, regardless of batch.

I have the feeling that much 2c-b HBr is mislabelled HCl for sales purposes.

atara said:
Well, yes, actually, but only if you have a significant quantity of the salt. NaBr is soluble in dry ethanol, whereas NaCl is not, so adding some NaBr to dry ethanol followed by the unknown form of 2C-B will create a precipitate if you have the hydrochloride, but not if you have the hydrobromide. Unfortunately this test requires ethanol with very little water content, I doubt everclear would work.
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Does the same apply to methanol? I have some sitting on a molecular sieve.
 
Anon0631 said:
Does the same apply to methanol? I have some sitting on a molecular sieve.
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I'm afraid not. NaCl is twenty times as soluble in methanol as in ethanol, so it will probably not precipitate as readily. You could see if NaBr dissolves in isopropanol, I have no data handy for that.

Nope. It's pertinent to wanting the HCl consistently from purchase to purchase so I can rely on dosing being the same, regardless of batch.
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Molar masses of the two salts differ by about 15%. That's not too much, but I understand your concern.

Also, I take it that 2C-B is going around on the street these days? Intriguing.
 
How is TLC going to help? Do you think the average person is going to have the time, skill, or effort to attempt column chromatography?

If OP wants to get 2c-B from a HBr to a HCl, salt, basify, extract with a nonpolar solvent, & add dry HCl.
 
Seriously though, I would just titrate my dose assuming that it is the HCl and compensate when needed at later attempts. Even when you know which salt it is you would need to apply that strategy anyway to make up for variance in purity!
But yes it is just my personal opinion that the compound is not strong or unsafe enough to call that margin a problem, and to warrant this - excusez-moi - pussyfooting.
 
Well this is interesting. I tested solubility of two different batches of supposed 2c-b HCl that I had knocking around. Both happily went into solution at 20mg/ml. I think that I can confirm from this that they are both in fact 2c-b HBr. Can someone weigh in with an opinion?

I wonder how much 2c-b HBr is mislabelled as HCl to make it a more desirable purchase?
 
2C-B HCl is not very soluble in water while the HBr salt is quite soluble maybe you can try to dissolve a bit in water and see if it dissolves very fast or slowly/not should be a quite good method.

but well anyway why you want to know? the ammounts of Br- is not worry-some its just a bit less potent by weight (~14% ) so just take the ammount if it is the HCl salt if it is to weak just do more next
 
Torabora said:
but well anyway why you want to know? the ammounts of Br- is not worry-some its just a bit less potent by weight (~14% ) so just take the ammount if it is the HCl salt if it is to weak just do more next
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Because if I've bought a quantity of 2c-b HCl but it turns out to be 2c-b HBr, then I've received less 2c-b than I've paid for.

Also this written by Shulgin, referring to the HBr salt if 2c-b:

There are many complicated salt forms, both polymorphs and hydrates, that can make the isolation and characterization of 2C-B treacherous. The happiest route is to form the insoluble hydrochloride salt by way of the free base.
Click to expand...

So presumably, it's not as simple as applying a simple multiplier to the dose. Each batch could be different.
 
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TLC does indeed seem to be the way to go, and it's not *that* out of reach for the sorts of people who will be discussing this thread. TLConscious is running a crowdfunding thing to get a load of kits to market too.

http://www.bluelight.ru/vb/threads/696366-REAL-testing-kits-Not-just-color-tests

I'd also like an easier way to test for the presence of the succinate counterion. 5-APB was sold as succinate for a long time and I suspect some of the HCl stuff still actually is succinate.
 
I've had 2CB HCl that deffinitely felt more than 14% stronger than the 2CB HBr I had, for what it's worth, it was also faster to come on. Over all I liked it better, honestly.
 
there is alot of factors that play into the purity and solubility of 2c-b, if you follow the synth, excess bromine can only be partially washed out of the 2c-b hbr product after bromination with cold acetic acid without huge loss in yield, imo you can only achieve 80-90% purity at this stage not factoring the weight of the hbr attachment. Now that will cause a dramatic variability in solubility properties. to achieve an isolated form of hbr the product must be freebased back into its oil form purified and then br2 added slowly in a chilled reaction vessel by titration.. now that is unnecessary imo and undesirable. so one must freebase the 2c-b hbr after bromination and DISTILL IT if this is skipped a huge portion of sids reaction products are salted out as well, if you take note 4-7g residue (cant remember) are left behind after distilling 31g or so in shulgins wirk. so once uou have your pure white oil you can salt to make the mostly insoluble hcl or if you desire a better on the nose product, then salt with fumaric>or acetic acid all three of which are very appealing crystals the hcl is tiny white and cubicle the fumaric is white fine crystals and acetic is yellowish and jagged my personal favorite.

Regards
Damn just realized this probably isn'tthe bestthread to go into such detail like that mods pleasecorrect me if need be.
but to contribute to the threads question there is a very easy way to test for the hcl just put a few drops if marquis reagent on it and if it fizzles or bubbles its the hcl :b
 
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Do you have anything to support the comment about HCl smoking? DXM.HBr smokes readily.

Do you mean just for 2C-B?

Could silver nitrate be of any use for detecting HCl salts?
 
sekio said:
the amount of base needed to titrate the salts to neutrality will be different
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Explain. Theres only a single amino group thats protonated in each salt, so the same amount of base is required to free the base.

Anon0631 said:
^ is there a way to predict how much of a NaOH solution at a certain concentration it will take to neutralise x mg of each salt?
Click to expand...

Yeah, its called stoichiometry. I'm pretty sure sekio has it wrong. Two equimolar (meaning they have the same number of molecules of acid) solutions of HCl and HBr will have the same pH since they're both strong acids. The only difference is their ability to protonate substrates but in this case the substrate can only be protonated by each acid at one atom. A simple test would be to add some of the salt to a test tube of hot concentrated sulfuric acid. If its the HBr salt, it'll turn orange. I think around 80% is a good concentration for the acid, there needs to be enough water in there to dissolve the HBr. Eventually the HBr will be oxidised so the solution will turn a reddish orange as Br2 is formed. The thing is though, if its only a mg that you add to the test tube, then you'd need a tiny amount of acid solution in order to be able to observe the color change. Maybe 0.1mL, I'm just guesstimating. I don't know if the drug would still be useable after the test, most likely not as the acid would oxidise it. BTW I wouldn't rely on solubility tests unless theres a very big difference in solubility.

Transform said:
Do you have anything to support the comment about HCl smoking? DXM.HBr smokes readily.

Do you mean just for 2C-B?

Could silver nitrate be of any use for detecting HCl salts?
Click to expand...

Yeah, you could add a small amount (too much and you'll have leftover unreacted silver nitrate so the results would be useless) silver nitrate, precipate out the halide salt then weight the precipitate. Siliver bromide is heavier so you could calculate which silver halide since you know how much silver nitrate you added. That would be a big hassle though.
 
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