Raspberry2-3-4

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

HerrHaber

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Is it possible to use Zirconium(II) hydride instead of NaBH4 for hydride reduction?
Raspberry2-3-4sounds 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

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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.
 

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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.
Raspberry2-3-4it'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

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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

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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.
Raspberry2-3-4so 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

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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.
CCL4 hufferThank you for your advice.
 

Raspberry2-3-4

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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

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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.
Raspberry2-3-4just follow a premade method if u want any yield i can tell u lack the expirience to "design" a synthesis so just follow procedures .
 
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