Smoking Toad Venom Phenomenon: Hamilton's Pharmacopeia Season 3

[ApeMaia]

First episode is out, an amazing story about Ken Nelson aka Albert Most, the person who first discovered in our modern era the psychoactive effects of 5-meo-DMT.
And there's a pretty neat video on the synth of the compound

h00ps://www.youtube.com/watch?v=fFXGa-Ruz_M&ab_channel=VICE

[bubbles]

Cool! I was looking forward to the new season.

Edit: I just watched it and it is indeed a very good episode! I'm not gonna spoil it but I really like what he did for 5-meo-dmt culture.

[loft]

Great to see the episodes being available for free. I hope this applies to the whole season!

FYI I attached the pages shown in the documentary added by Hamilton Morris. Did anyone find a place to buy this reissued pamphlet?

[bubbles]

https://www.psychedelictoadofthesonorandesert.com/

Not working yet but should be later today according to Hamilton.

[loft]

I wonder why Hamilton cited He and Xi (https://sci-hub.st/https://www.sciencedirect.com/science/article/abs/pii/S0040403914008521), although they themselves referenced Bosch et al.'s paper as the origin for the reductive amination (https://sci-hub.st/https://www.sciencedirect.com/science/article/abs/pii/S0040402000010917).

Taken from Bosch et al.:

3-[(2-Dimethylamino)ethyl]-5-(1-pyrrolidinylsulfonylmethyl)indole (9b). A solution of 35% formaldehyde (35 mL,  416 mmol)  in  MeOH  (35 mL)  and  a  solution  of NaBH4 (5 g, 132 mmol) in H2O (70 mL) were added drop-wise, simultaneously, at 15°C to a well-stirred solution of tryptamine (8.1 g,  26 mmol)  in  MeOH  (150 mL).  The mixture  was  stirred  at  15°C  for  0.5 h,  2N  aqueous  HCl was cautiously added to bring the pH to 3, and the resulting mixture was stirred for 10 min. Then, the pH was adjusted to 6.5±7 with saturated aqueous NaHCO3, MeOH was evaporated,  and  H2O  (50 mL)  was  added.  The  mixture  was washed  with  EtOAc  (2x 150 mL),  basified  with  K2CO3, and   extracted   with   EtOAc   (2x 130 mL).   The   organic extracts  were  dried,  filtered, and  concentrated  to  give 9b (7.70 g, 88%) as a brown solid.

From He et al (Supplementary), a more closely related structure, DMT itself:

DMT (9). A solution of 37% formaldehyde (147.0 ml, 2000.0 mmol) in MeOH (80.0 ml) and a solution of NaBH4 (23.6 g, 625.0 mmol) in H2O (210.0 ml) were added dropwise, simultaneously,  at 15 °C to a well-stirred solution of tryptamine (20.0 g, 125.0 mmol) in MeOH (320.0 ml). The mixture was stirred at room temperature for 30 min. Then , the solution was adjusted to pH 9 by addition of 10% aqueous Na2CO3. MeOH was removed by distillation and the product was extracted with ethyl acetate (3×100 ml). Then the organic layer was washed with brine, dried over Na2SO4, concentrated under reduced pressure. The residue was recrystallized with ethyl acetate-hexane (5:1) to give 9 as a light brown solid (yield 21.2 g, 90.2%).

It's been a while since I looked at 1H NMR spectra but the one from DMT, synthesized as described above by He et al., is attached below.

Final edit to this post: I'm just writing down the CC from Hamilton's synthesis

100 grams of 5-MeO-tryptamine freebase is dissolved in MeOH with vigorous magnetic stirring. A thermometer probe is inserted into the methanolic 5-MeO-tryptamine, and the solution is cooled until it nears 0 °C. Aq. KOH is used to dissolve and stabilize 100 grams of NaBH4, and the solution is transferred into an addition funnel. A second addition funnel is charged with a MeOH-stabilized aq. 37% formaldehyde solution, and the drop-wise addition begins. "And now I start adding the borohydride." [...] Borate salts gradually precipitate, and the salt volume is reduced by overnight heating. As the methanol evaporates, 5-MeO-DMT precipitates as a brown oil and coalesces on the surface. "Pretty beautiful." Simple distillation is used to strip the remaining water, followed by purification of the crude freebase via short path vacuum distillation, "We did it. Yes.", and recrystallization. [...] After TLC had shown total transformation of the starting material, LC-MS confirmed the product was 5-MeO-DMT.

[ApeMaia]

DMT (9). A solution of 37% formaldehyde (147.0 ml, 2000.0 mmol) in MeOH (80.0 ml) and a solution of NaBH4 (23.6 g, 625.0 mmol) in H2O (210.0 ml) were added dropwise, simultaneously,  at 15 °C to a well-stirred solution of tryptamine (20.0 g, 125.0 mmol) in MeOH (320.0 ml). The mixture was stirred at room temperature for 30 min. Then , the solution was adjusted to pH 9 by addition of 10% aqueous Na2CO3. MeOH was removed by distillation and the product was extracted with ethyl acetate (3×100 ml). Then the organic layer was washed with brine, dried over Na2SO4, concentrated under reduced pressure. The residue was recrystallized with ethyl acetate-hexane (5:1) to give 9 as a light brown solid (yield 21.2 g, 90.2%)..

[/quote]

Oh man that 90,2% surely looks good. I know it's a bit late but i'm texting Santa right now to deliver me a 5-10Lt glass reactor

[Sawdust and Honey]

I watched the episode.
Absolutely amazing work on behalf of Hamilton and his team. I don't care what VICE is, what they do or did - this is one of the best, if not the best existing chemistry related shows. It made my blood boil to see these idiot braincooked spiritualists claiming that they're "natural people".

Now, we should adapt this synthesis not to include a vacuum distillation, as this is only possible in large scale production and is inconvenient. Maybe fumarate salt once again would do the trick? The workup would be - use enough methanol to keep the borate salts inside, extract with acetone or chloroform, precipitate the fumarate salt using FASA.

[ApeMaia]

i'm texting Santa right now to deliver me a 5-10Lt glass reactor

It's REACTOR TIME ! Just found a Chemglass 5lt used one, looks a beauty. plus i already got the short path distillation thingie because a friend does CBD distillation, and he got 1 to spare fooooor sure

Now all i need is a fine Mexican lady to help me out and yell me CABRRRROOOON NOONOOO NOOOO if i start fucking up something

I watched the episode.
Absolutely amazing work on behalf of Hamilton and his team. I don't care what VICE is, what they do or did - this is one of the best, if not the best existing chemistry related shows. It made my blood boil to see these idiot braincooked spiritualists claiming that they're "natural people".

Now, we should adapt this synthesis not to include a vacuum distillation, as this is only possible in large scale production and is inconvenient. Maybe fumarate salt once again would do the trick? The workup would be - use enough methanol to keep the borate salts inside, extract with acetone or chloroform, precipitate the fumarate salt using FASA.

Eh, you know the woke/crystal therapy people, they think it's good only if you squeeze a poor toad or cut down 99% of the cacti population in order to juice them.

[RhinoJackson]

Good first episode!
Now Hamiltion just needs to make some synthetic toad soul to sell the spiritualists...

[loft]

I enjoyed his reaction and mimic when that question arised. I mean it was 100% sure to come. And I was confronted with this opinion in the past too, I guess most of us were. It's just a hopeless discussion.

[foroz]

I have tried to view this from europe australia asia south america africa.

only ip sets that work are the usa so for those not in the usa set your vpn to a usa server to get it to work

[Sawdust and Honey]

Or just watch it on bitchute: hxxps://www.bitchute.com/video/SHtgUagKk0hp/

[Sawdust and Honey]

Has anyone been able to scan the pamphlet and share it? I wanted to buy it myself, but it's already sold out.

[stoichiometric_steve]

100 grams of 5-MeO-tryptamine freebase is dissolved in MeOH with vigorous magnetic stirring. A thermometer probe is inserted into the methanolic 5-MeO-tryptamine, and the solution is cooled until it nears 0 °C. Aq. KOH is used to dissolve and stabilize 100 grams of NaBH4, and the solution is transferred into an addition funnel. A second addition funnel is charged with a MeOH-stabilized aq. 37% formaldehyde solution, and the drop-wise addition begins. "And now I start adding the borohydride." [...] Borate salts gradually precipitate, and the salt volume is reduced by overnight heating. As the methanol evaporates, 5-MeO-DMT precipitates as a brown oil and coalesces on the surface. "Pretty beautiful." Simple distillation is used to strip the remaining water, followed by purification of the crude freebase via short path vacuum distillation, "We did it. Yes.", and recrystallization. [...] After TLC had shown total transformation of the starting material, LC-MS confirmed the product was 5-MeO-DMT.

There sadly is some stuff missing in that synthesis, first of all if he uses Acetone/dry ice as his bath, then the reaction most likely will run below 0°C. Doesn't mention reaction time or amount of HCHO. Simple distillation may or may not carry along freebase 5-MeO-DMT. Also a bit puzzled how he can reduce salt volume by heating, probably meant to say solvent volume.
Not the most efficient or clever workup, but if it works, it's not stupid, right?

[carl]

*cough cough*

[foroz]

100 grams of 5-MeO-tryptamine freebase is dissolved in MeOH with vigorous magnetic stirring. A thermometer probe is inserted into the methanolic 5-MeO-tryptamine, and the solution is cooled until it nears 0 °C. Aq. KOH is used to dissolve and stabilize 100 grams of NaBH4, and the solution is transferred into an addition funnel. A second addition funnel is charged with a MeOH-stabilized aq. 37% formaldehyde solution, and the drop-wise addition begins. "And now I start adding the borohydride." [...] Borate salts gradually precipitate, and the salt volume is reduced by overnight heating. As the methanol evaporates, 5-MeO-DMT precipitates as a brown oil and coalesces on the surface. "Pretty beautiful." Simple distillation is used to strip the remaining water, followed by purification of the crude freebase via short path vacuum distillation, "We did it. Yes.", and recrystallization. [...] After TLC had shown total transformation of the starting material, LC-MS confirmed the product was 5-MeO-DMT.

There sadly is some stuff missing in that synthesis, first of all if he uses Acetone/dry ice as his bath, then the reaction most likely will run below 0°C. Doesn't mention reaction time or amount of HCHO. Simple distillation may or may not carry along freebase 5-MeO-DMT. Also a bit puzzled how he can reduce salt volume by heating, probably meant to say solvent volume.
Not the most efficient or clever workup, but if it works, it's not stupid, right?

watch it again.

he is adding dry ice cubes one or two at a time.

just because your using dry ice does not mean your reaction temp is below 0C

it all depends on volume of solvent reaction exotherm and how much dry ice to acetone there is.

he is probably just being lazy as it is easier to use a couple of dry ice cubes in acetone than an ice bath to keep an exothermic reaction

around 0 too 5C.

it also allows you to increase your addition speed.

tryptamine does not azeotrope with methanol.

methanol does not azeotrope with water and as you remove the methanol the salts will dissolve.

and finally the synth he is doing is well known so really he doesn't have to put everything down for a chemist to do it.

after all its just entertainment rather than a journal paper.

please don't pick on noobs its not becoming of you.

[stoichiometric_steve]

unsurprisingly, you missed the entire point i was making.

[bubbles]

*cough cough*

hxxps://www.youtube.com/watch?v=SQEhBai711o

[foroz]

I am going to ask you this one more time and then I am going to ask that something be done about it.

my views on here have nothing to do with other forums so stop trying to bring them up.

I am at the moment doing an important project that has taken a lot of time coding.

the time I spend in other places also takes a lot of time and I do not have unlimited time.

I am welcome where ever I go as my skill set is of use so stop trying to imply that you can bully me or decloak me or what ever you are trying to say.

if you have a criticism on what I put up here by all means state you piece but I am not going to tollerate you bringing up other forums here.

[carl]

Pull yourself together guys, take it elsewhere or talk it out in private!
Both of you, none of you are the better with your private feud here!