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N&PD Moderators: Skorpio | someguyontheinternet
Anyone know if ecstasy contains sulfur?
- Thread starter Ninjetic
- Start date
szuko000
Bluelight Crew
Pure MDxx would not contain sulfur. I do believe sulfuric acid is used in its synthesis but a good chemist should be able to remove most of not all sulfur containing impurities. Theres also a chance of amphetamine sulfate in your pills. I dont know of any way to test for sulfur if you are allergic i wish i could help.
Zzyzx
Bluelight Crew
With high end laboratory equipment maybe.. But unless you are severly allergic to those compounds than there is nothing to fear. Seriously its the first time I hear about sulfur compounds in a pill.
poopstation
Bluelighter
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- Oct 13, 2009
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- 375
the only mdma synthesis that uses h2so4 is one of the reactions in the peracid oxidation procedure. the pinacol-pinacolone rearrangement of isosafrole epoxide/glycol into mdp-2-p. even then, h2so4 can be substituted with hcl for higher yields because hcl is gentler on the sensitive md-molecule. even after the reaction is complete, the h2so4 is easily neutralized and removed via the standard basic h2o washes during the work-up. then the ketone is vacuum distilled, so no there is no way sulfur is going to be in the final product. but i just wanted you to know that there is only one route i'm aware of using h2so4 and there is no way in hell it can make it to the final product. even if NO washes and NO distillation were done then the aminative reduction (which has a high ph due to MeAm) would fail leading to zero product. so even if h2so4 is used it will not make it to the end product due to neutralization and solubility differences between it and the desired precursor oils.
h2so4 is not a preferred strong acid with mdma because it has the reputation of cleaving the methylenedioxy ring lowering yields. think of the reagent tests you guys use and look for the purple/black reaction, that is the h2so4 cleaving the md ring.
a person can opt for mdma sulfate instead of mdma hcl but that would be a mere novelty, i've never seen the sulfate salt of mdma and doubt you ever will either. hcl is the industry standard, even in pharmaceuticals. amphetamine is common in the sulfate salt only because the hcl salt of amphetamine is hygroscopic. also keep in mind that pills can of course be adulterated with God knows what... by some crazy middleman asshole, but i just wanted you to know that no sulfur compounds will be in the product as part of the synthesis.
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phase_dancer
Bluelight Crew
An authorised uni project I did some years ago involved producing the ketone from iso using the peracetic acid route. H2SO4 was used in preparation of the peracid, and to open the formed epoxide ring. The reaction was intentionally run longer to look for overoxidation products. While piperonal was a major impurity, analysis (GC/MS, NMR ) showed no compounds present with a cleaved methylenedioxy ring.
As for sulphur: I agree with poopstation that it's unlikely MDMA itself would be contaminated with sulphur, but it can't be ruled out completely as routes employing alkyl tosylsulfonate intermediates are known. Also, a bisulfite adduct can be prepared to purify the ketone. While it's unlikely there would be residual sulfur present in the final product of such syntheses, there's always the possibility of contamination.
As for sulphur: I agree with poopstation that it's unlikely MDMA itself would be contaminated with sulphur, but it can't be ruled out completely as routes employing alkyl tosylsulfonate intermediates are known. Also, a bisulfite adduct can be prepared to purify the ketone. While it's unlikely there would be residual sulfur present in the final product of such syntheses, there's always the possibility of contamination.
poopstation
Bluelighter
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- Oct 13, 2009
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- 375
phase_dancer i must say i've been admiring your posts for many years. thanks for the correction and education.
your gc/ms results are interesting. i've heard from bees for a long time that h2so4 is notorious for ring cleavage, i could've sworn that even rhodium himself stated this although my memory might be incorrect. i've read about some strange methoxy by-products but again it's going off memory and don't have publications on hand to support that claim so perhaps i misread it and those by-products are due to impurities present in the samples used rather than being blamed on the h2so4.
so piperonal is the primary by-product of peracid method? how does that occur? what compound is the isosafrole over-oxidized to past the glycol ester that is then dehydrated to the aldehyde (assuming that is indeed what happens)? i always thought it was un-isomerized safrole that was oxidized to the aldehyde and responsible for the piperonal?
this would certainly explain the large jump in yields as reported by buffering the reaction, which limits the oxidation product to the epoxide or at most - the glycol and not the glycol ester - hence less over-oxidation.
if this is starting to cross the lines on bluelight allowed discussion, would you mind PM'ing me? you just rocked my world with that information and being that it's coming from you, i'm going to lean towards you being correct over what i've been told.
your gc/ms results are interesting. i've heard from bees for a long time that h2so4 is notorious for ring cleavage, i could've sworn that even rhodium himself stated this although my memory might be incorrect. i've read about some strange methoxy by-products but again it's going off memory and don't have publications on hand to support that claim so perhaps i misread it and those by-products are due to impurities present in the samples used rather than being blamed on the h2so4.
so piperonal is the primary by-product of peracid method? how does that occur? what compound is the isosafrole over-oxidized to past the glycol ester that is then dehydrated to the aldehyde (assuming that is indeed what happens)? i always thought it was un-isomerized safrole that was oxidized to the aldehyde and responsible for the piperonal?
this would certainly explain the large jump in yields as reported by buffering the reaction, which limits the oxidation product to the epoxide or at most - the glycol and not the glycol ester - hence less over-oxidation.
if this is starting to cross the lines on bluelight allowed discussion, would you mind PM'ing me? you just rocked my world with that information and being that it's coming from you, i'm going to lean towards you being correct over what i've been told.
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phase_dancer
Bluelight Crew
^ Bit busy today, I'll PM when I get the chance
poopstation
Bluelighter
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- 375
thanks for your time and so sorry to derail the thread but at least the OP's question was answered before my derailing 
MazDan
Bluelight Crew
Im going to send this over to Advanced drug Discussion.
The mods over there understand this stuff far better than I however they may feel it necessary to remove or edit sdome of the discussion due to our synthesis discussion rules.
Im no expert but they are.
The mods over there understand this stuff far better than I however they may feel it necessary to remove or edit sdome of the discussion due to our synthesis discussion rules.
Im no expert but they are.
This is nit-picky of me, but you can't just be categorically allergic to the sulfur atom; you'd have no body.
Usually the allergy is to the sulfonamide functional group.
In which case MDMA should be safe, since it has nothing like that in it, and i cannot fathom a way to get a sulfonamide out of anything close to an MDMA synth. That's assuming you get real MDMA, which is not really a safe assumption without testing.
Actually though... are there any recreational drugs that contain sulfonamide groups? Are there any that are organosulfur compounds at all, other than the 2C-T-#s, and a few other weird ones Shulgin made?
MurphyClox
Bluelighter
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- Mar 26, 2008
- Messages
- 1,416
The opening question is kinda...questionable. ![:\](https://bluelight.org/xf/BL_Images/Orig_Emoji/wrygrin.gif "wry grin :\")
Well, anyway: The presence of sulfur, bound in any way (eg. sulfonamides, sulfides, disulfides etc.) can be checked easily with the elemental analysis method acc. to Lassaigne. "Easily" includes in this case the availability of metallic sodium, among other reagents.
As this is no synthesis but rather analytics, I provide the procedure in short:
1. Place in a small combustion tube a finely powdered sample of your substance/drug, around 20-5 mg.
2. Place a small piece of blank sodium metal above, in such a fashion that the metal does not touch the sample.
3. Heat carefully (fumehood! protection googles!!!) with the reduced flame of a Bunsen burner, so that you do not carbonize the sample but simply melt the sodium. It should run down as droplet. (melting point of sodium = ca. 98 °C)
4. When the liquid sodium meets the sample, turn on the Bunsen burner to full power and heat for at least one minute. The whole tube should be glowing red for 2-3 min!
5. Let the whole tube drop into a reagent tube with cold, destilled water. The combustion tube should crack instantly. (Googles!!!)
6. Filter the solution (careful! it's quite alkaline), and wash the filter throuroughly with water. The final volume should not excess ca. 10-15 ml.
7. From this solution one can detect sulfur (as sulfide) by adding some drops of a 2.5% solution of sodium pentacyanonitrosylferrat. A positive test yields a violett coloration.
This method is quite reliable and can detect sulfur in practically all compounds, bound covalently or ionic.
There's one hitch: Obtain sodium metal.
- Murphy
Well, anyway: The presence of sulfur, bound in any way (eg. sulfonamides, sulfides, disulfides etc.) can be checked easily with the elemental analysis method acc. to Lassaigne. "Easily" includes in this case the availability of metallic sodium, among other reagents.
As this is no synthesis but rather analytics, I provide the procedure in short:
1. Place in a small combustion tube a finely powdered sample of your substance/drug, around 20-5 mg.
2. Place a small piece of blank sodium metal above, in such a fashion that the metal does not touch the sample.
3. Heat carefully (fumehood! protection googles!!!) with the reduced flame of a Bunsen burner, so that you do not carbonize the sample but simply melt the sodium. It should run down as droplet. (melting point of sodium = ca. 98 °C)
4. When the liquid sodium meets the sample, turn on the Bunsen burner to full power and heat for at least one minute. The whole tube should be glowing red for 2-3 min!
5. Let the whole tube drop into a reagent tube with cold, destilled water. The combustion tube should crack instantly. (Googles!!!)
6. Filter the solution (careful! it's quite alkaline), and wash the filter throuroughly with water. The final volume should not excess ca. 10-15 ml.
7. From this solution one can detect sulfur (as sulfide) by adding some drops of a 2.5% solution of sodium pentacyanonitrosylferrat. A positive test yields a violett coloration.
This method is quite reliable and can detect sulfur in practically all compounds, bound covalently or ionic.
There's one hitch: Obtain sodium metal.
- Murphy
MurphyClox
Bluelighter
- Joined
- Mar 26, 2008
- Messages
- 1,416
I'll take care, in case the last post was adressed to me.
The described method can hardly considered as synthesis, as all compounds will just get degraded under such harsh conditions. One can not synthesize anything useful with this procedure.
- Murphy
The described method can hardly considered as synthesis, as all compounds will just get degraded under such harsh conditions. One can not synthesize anything useful with this procedure.
- Murphy
phase_dancer
Bluelight Crew
^ mmm..Nuke, not wishing to ruffle any feather here, but that stuff was posted in response to earlier posts, before the thread was moved here. Quite surprised you'd be upset by this as afterall, we are talking about impurities. Correct me if I'm wrong but don't the guidelines here permit synth talk in such cases.