5-MeO-Tryptamine Synthesis From Melatonin

[csigger]

What can replace n-butanol?
Thanks

 

[CCL4 huffer]

isobutanol worked for me

 

[OneTensionSkyRed]

Benzyl alcohol with ethanol or methanol to dissolve NaOH works okay for this. Isopropyl alcohol can also be used although the reaction will take much longer time to complete. Maybe even glycerine+ethanol/methanol can be used for this.

 

[Plantguy]

Can anything else than n butanol work

 

[Raspberry2-3-4]

Is it possible to use Zirconium(II) hydride instead of NaBH4 for hydride reduction?

 

[HerrHaber]

sounds exotic therefore I have no clue but you should check a similar procedure to a known Na borohydride prep then compare conditions to have an idea of the needed data in order to approach this

 

[Raspberry2-3-4]

I made a big mistake. I thought I was using butanol, but ended up using methanol instead. I realized my mistake after heating and stirring for 2 hours, and when I left it to cool, it solidified into a gel-like consistency. Methanol was added, stirred, concentrated using the same procedure as when using butanol, and crystallized after cooling. Yield is poor.

 

[HerrHaber]

it's how we learn and implement knowledge... things don't typically work from the first try, having it working but very inefficient is what you are normally getting before exploring the reaction. I feel like I'm willing to give it a try with IPA instead of butanol (aware of the miscibility), I am somewhat puzzled by the use of dithionite (in the original rhodium writeup) and plan to add a little NaBH4 to keep the mixture in reducing medium.

 

[Raspberry2-3-4]

Is there anything wrong with the flow from the generated 5meo-T in the following method?
Here are the steps to extraction.


1:
4.7 grams of 5Mmeo-T was dissolved into 100 ml of methanol,
which was cooled to 0° C. in an ice-salt bath.

2:
Add 3.70 ml of acetone to the stirred methanol, After 15 minutes, 1.45 g of NaBH4 was added slowly to keep the solution below 5°C. This was stirred in an ice bath for 60 minutes.

3:
After 60 minutes, it was stirred in a 35 °C water bath to quench the NaBH4 .

4:
Cool the methanol back to 0°C, 0.75g of para-formaldehyde solution were added. After 15 minutes, slowly adding 0.65 g of NaBH4. After 60 minutes, it was stirred in a 35 °C water bath to quench the NaBH4

5:
After addition, it was stirred at room temperature for 48 hours.

 

[CCL4 huffer]

so to start off why the acetone?
seccondly i dont think paraformaldehyde would work.
also wtf why are u making it so complicated why step 3??????????
clearly if ur quenching it in the end why would u need to quench it before u do realise that the cold temperatures are partly there to make it interact less with the formalin also not to mention since when does heat quench NaBH4 u didnt add any warter or anything that i see that it could reakt with.
oh also another thing i doubt a ice salt bath would do the job since u need under -15
just go follow this method https://bbgate.com/threads/synthesis-5-meo-dmt-from-5-meo-tryptamine.294/
ur just wasting chemikals with that.
oh also another thing i doubt a ice salt bath would do the job since u need under -15.

 

[Raspberry2-3-4]

Thank you for your advice.

 

[Raspberry2-3-4]

I haven't worked out the details of the process after the reaction is complete, but I'm thinking of it as follows.

1:
Add HCl until the pH of the mixture is about 3 and evaporate the methanol (preferably under vacuum)

2:
The remaining mixture is then washed 3 times with 50 mL DCM and the DCM is discarded/reused.

3:
NaOH is then added to the aqueous solution until the pH is approximately 10 and the solution is again washed 3 times with 50 mL DCM, collected and stored. Dry DCM with MgSO 4 and evaporate DCM.

 

[CCL4 huffer]

just follow a premade method if u want any yield i can tell u lack the expirience to "design" a synthesis so just follow procedures .

 

[hu1984915]

Anyone konws how to synthesis 5meo-dipt from 5-meo-tryptamine?

​

 

[CCL4 huffer]

isopropyl iodide ig

 

[hu1984915]

proceed with the synthesis directly?
Do you have a tutorial link
ty

 

[hu1984915]

em....
it seems generate nipt not dipt?

 

[CCL4 huffer]

just do the shulgin methyl iodide synthesis but substitute the methyl iodide with isopropyl iodide