AL-LAD Mass Spectrography and 1H-NMR results

[Rorthron]

[I hope I'm not breaking the rules of ADD, I read the rules and I saw nothing against it. Plus I've seen similar posts here. However, on any case if this should not be here, please advise]

So, I'm trying to make sense of this information. Apparently AL-LAD is in the market and some vendors have provided Mass Spectrography and NMR images:

As far as I can tell and comparing to this, at least the 1H NMR looks like an ergolide, but in fact I do not have the analytic background to assess it, and I do not know how to interpret at all the MS results.

Thanks for your help,

 

[sekio]

The MS checks out, AL-LAD has a mass of 349.22 and approx 25% 350.22. Since it's likely a LC-MS and it's in positive mode the peak at 350/351 is AL-LAD+(H⁺)

It's not possible to tell if it's 100% pure with a baseline like that though... I'd bet it's safe to say probably upwards of 70%.

 

[Torresmo]

AL-LAD NMR spectogram

Same question here, I inquired a vendor and he sent me this NMR spectrogram, which he says is from the last batch (coincidentally [?], one day after the first post here). Can someone, please, tell me if this is AL-LAD?

 

[Hyperthesis]

Compare it against the 1H NMR spectrum in the opening post and you'll at least notice that it is not the same. I can tell you furthermore that it's not AL_LAD.
Apart from this is the quality of the spectrum just crappy:
Why is the integral missing for some signals (e.g. at 1.9 ppm or 2.25 ppm)?
Why are there no chemical shifts given?
How are we supposed to interpret the spectrum without a magnification? At the given resolution I can not tell for sure if the signals between 6.5-7.5 ppm are triplets, doublets or something else; in the aliphatic range its even worse.

Spectrum interpretation goes tasseography, hooray!

 

[Torresmo]

Compare it against the 1H NMR spectrum in the opening post and you'll at least notice that it is not the same. I can tell you furthermore that it's not AL_LAD.
Apart from this is the quality of the spectrum just crappy:
Why is the integral missing for some signals (e.g. at 1.9 ppm or 2.25 ppm)?
Why are there no chemical shifts given?
How are we supposed to interpret the spectrum without a magnification? At the given resolution I can not tell for sure if the signals between 6.5-7.5 ppm are triplets, doublets or something else; in the aliphatic range its even worse.

Spectrum interpretation goes tasseography, hooray!

Haha, thanks for your feedback!
Sorry but, i had no idea on how to intepret this, although visually it is clearly different...
Anyway, i should have posted this before: the guy told me e had 5kg in stock, and other things which made me notice it is just a laughable scam...

 

[kman1898]

The MS checks out, AL-LAD has a mass of 349.22 and approx 25% 350.22. Since it's likely a LC-MS and it's in positive mode the peak at 350/351 is AL-LAD+(H⁺)

Source for legitimate AL-LAD MS? I've talked with Dr. Nichols and he doesn't have the relevant data, you seem to have, anymore.

All of the lab notebooks, spectra, etc., for our compounds were either discarded or put into storage in the Purdue Archives after I retired. I don’t know what kind of mass spec they ran, but the M+H peak would be at m/z 336.

Would love to see some credible spec data that we can actually compare this too. Never seen anything legitimate anywhere though :/

 

[sekio]

Source for legitimate AL-LAD MS? I've talked with Dr. Nichols and he doesn't have the relevant data, you seem to have, anymore.

Don't have any. But I can draw AL-LAD in Chemdraw and get the mass.

 

[Zeds(NCO2CH2CH3)2]

Hi all two problems, if I we believe the mass above then it is freebase al-lad which is poorly absorbed. If they didn't make it into a tartrate salt then wtf.. They are idiot China chemists or they don't care about making more $ by buffering the mw(adding mass ala salt) then claiming original mw and just selling it by the kilo....

Major problem number two, the 1H at appx 10.7, indole hydrogen is never there and this suggests an aliphatic amide with one alkylation.. The Molecular weights which match(off of the top of my head appx calculation) are N-butyl AL-LAD and n-isopropyl AL-LAD... Freebase..

Which might actually be legal.. It deserves a good hard look OK because China may be trolling the analogue act more than we realize... But are somehow smart enough to produce ms data that is almost believable..

Zedsdead

 

[pr0d1gy]

Hi all two problems, if I we believe the mass above then it is freebase al-lad which is poorly absorbed. If they didn't make it into a tartrate salt then wtf.. They are idiot China chemists or they don't care about making more $ by buffering the mw(adding mass ala salt) then claiming original mw and just selling it by the kilo....

Major problem number two, the 1H at appx 10.7, indole hydrogen is never there and this suggests an aliphatic amide with one alkylation.. The Molecular weights which match(off of the top of my head appx calculation) are N-butyl AL-LAD and n-isopropyl AL-LAD... Freebase..

Which might actually be legal.. It deserves a good hard look OK because China may be trolling the analogue act more than we realize... But are somehow smart enough to produce ms data that is almost believable..

Zedsdead

I disagree, the HNMR does appear to be that of AL-LAD. The chemical shift of the indolic N-H is as would be expected in DMSO-D6. The provided MS supports the assumption of AL-LAD although both the LC?MS and HNMR show some noticeable impurities.

Thanks to the OP for posting this data.

 

[vecktor]

Hi all two problems, if I we believe the mass above then it is freebase al-lad which is poorly absorbed. If they didn't make it into a tartrate salt then wtf.. They are idiot China chemists or they don't care about making more $ by buffering the mw(adding mass ala salt) then claiming original mw and just selling it by the kilo....
Zedsdead

Eh? of course it will be freebase coming out the end of an HPLC column, the eluent is buffered, any tartarate or maleate or whatever counter ion will be separated it is not going to magically elute at the same time, recreating the original salt complete with its original counterion. even if it did the MS skimmer would remove the oppositely charged counterion and the msd wouldn't see it

As for idiot chinese chemists? who the hell do you think makes all the generic pharms and everything that has kept you alive up to this point.

No comment with respect to the NMR.