Meskalinsyntese med nitromethan. 1000g skala.

[Mr Gonzo]

Hej med hensyn til LAH, er der noget andet, der er lettere at få fat i og bruge i stedet, eller er der en måde, hvorpå jeg kan blive instrueret i, hvordan jeg køber hydrid fra et sted med minimalt besvær? Prøvede et sted i Indien, og de havde ikke noget af det! Jeg er baseret i Storbritannien

 

[FredDurst]

Fik du fat i nogle til Storbritannien i sidste ende?

 

[Field7]

I was afraid of LAH, too, but I got over it.

1) Bake your glassware, so it's dry.

2) Use *anhydrous* THF from a reputable source.

3) Make your addition slowly, and allow each portion to react a bit before adding the next portion....swirl...

4) REMEMBER nothing will burst into a firey ball of HOLY-FUCKING-SHIT if your solvent is well below the flash point temperature; which is why you perform your additions in an ice water bath.

5) Use a drying tube when you run the reaction.


Warning:
Don't perform this reaction poolside, or in a damp cave. If running this reaction at room temperature, do not spit, pee, or ejaculate into it as it may get very angry, very fast. That, and it'd just be gross.

 

[Rabidreject]

Ha that’s a good reply.
yeah I never got over my feelings about LAH so far as I was able to figure out the copper/NaBh4 reduction. I even bought a bottle of THF for that purpose.

it makes sense about keeping it way below the flash point yeah. And I’ll save my masturbation for reactions that don’t use anhydrous conditions ha

 

[Field7]

I save mine mine in a bottle on my nightstand. Right under the black light.

Yeah, anhydrous, and below flash point. Also, even with Sodium Borohydride reduction system (+Copper, or Tin Chloride etc), It seems that performing the additions at low temperatures makes a significant difference.

ALSO... and this is an educated guess...I think folks may have it backwards(ish). I think, in the case of a styrene, you'd want to add the copper first, and let it stir a while...

 

[malesh67482]

Does this synthesis work for 2,5 dimethoxbenzaldehyde? Is the reduction using NaBh4 and copper chloride still the best way for reduction? And then the cleanup using oxalic acid?

 

[HIGGS BOSSON]

Yes

 

[Rabidreject]

Yeah, I didn’t even use the oxylate, I just made the sulfate salt and then used that to do an aromatic electrophillic substitution

 

[Field7]

Like HIGGS said--- yes. It'll work for that.

Tin Chloride keeps popping up in related literature, too, as do copper nanoparticles.

In chemistry, as in life, there are options...

 

[Rabidreject]

Yes, is a great way to reduce nitroalkene’s. From what I understand it’s just 4-haloginated aldehyde’s that it kicks off, which is why people tend to brominate or iodinate or whatever from 2c-h

 

[Field7]

I'd like to see more on bromination without elemental bromine.

 

[William D.]

HBr or KBr

 

[Hest]

For the synthesis of the aldehyde I prefer this one ....

3,4,5-Trimethoxybenzaldehyde Synthesis - [www.rhodium.ws]

 

[Rabidreject]

Yeah that looks good but I’m lazy so I just bought the aldehyde!

 

[William D.]

I advise you to use LAH, if possible. Products of this class in my opinion are better with this method.

 

[Rabidreject]

Oh really? In terms of what yield? Or do you mean qualitatively?
I do have all necessary items…and I do also need to reduce some more 2,5-DMONS and got a pretty bad yield from boro last time. Maybe maybe

 

[Hest]

Haha, Well that is preferred method number one

In some countries it's quite reguleret

 

[Rabidreject]

Oh interesting. Yeah I always thought it was a bit of a gap in their pointless efforts to control precursors!

 

[Hest]

I guess 345-TMBA is special. Here in Denmark its a class 1a (highest class) substance. Same class as Heroin.
I can't imagine the marked for mescaline in Denmark be very big, so it's kind of pointless. Nevertheless wort full to remember if one is walking around with 100g 345-TMBA

 

[Rabidreject]

Yeah fair enough.
I take it 2,5-DMOBA is the same?

 

[Hest]

I take it 2,5-DMOBA is the same?

Nope, only 345. I think it's some kind of leftpwer from the 80 in the Danish Law.