Syntheses of 2C-phenylethylamines

[Sonnettales]

I am currently in the middle of a 2c-b synth and I’ve encountered a directive that says

“A 250 mL RB flask was charged with 16.6 g 2,5-dimethoxybenzaldehyde,
1.6 g NaOAc and 50 mL nitromethane. Refluxing for 4h yielded 14.4 g of the corresponding nitrostyrene [1] after recrystallization.
5.0 g of 2,5-dimethoxylphenyl-2-nitroethene was added to a solution of 4.0 g sodium borohydride in 100 mL isopropanol. This yielded 4.2 g of a yellow oil
after decomposition of the excess borohydride followed by the usual work-up (B).
The 2,5-dimethoxyphenyl-2-nitroethane was dissolved in 100 mL isopropanol with 8 molar equivalents Zn and 3.5 molar equivalents HOAc (relative to amount of Zn). This yielded 2.0 g of 2,5-dimethoxyphenylethylamine as a faintly yellow oil (C).

I need help with the sentence I’ve underlined. What exactly does this mean. Before I started, I took it to mean the oil would be washed with acetic acid and separated via sep funnel. Now that I am in the middle of the synth I am not so sure. I would appreciate any help I can get from anyone on this.

 

[w2x3f5]

usually, excess borohydride is decomposed with acid and salts are filtered off.

I'm worried about why sodium acetate is used in the Henry condensation and I don't understand why you first restore the double bond and then restore the nitro group separately. Styrenes are reduced on zinc in hydrochloric acid (double bond and nitro group), this does not work for nitropropenes.

or you can use sodium borohydride with a copper catalyst

 

[Sonnettales]

Hey w2x3f5, thank you for the reply. It was one of those things I needed to be sure. And I appreciate the concern. I’m not sure exactly what you mean by “restoring the double bond and the nitro separately.” The NaBH4 reduces the double bond and then the zinc in acetic acid reduces the nitro group. Maybe since that’s the difference that’s why there’s no restoring of any double bonds ie oxidation going on. I’m tryin real hard to attach a file but I am unable. If you have a wickr account or proton mail I can send it to you like that. I can also let you know how it turns out. I have other work ups but I wanted to try this one since it theoretically only gives about 2 grams of final product and I thought it would be interesting if it worked. I realize I’m not using LAH and that’s intentional. The manuscript starts with anise oil which is what I started with. The hardest chem to get for that part of the work up was potassium dichromate. Had to order it from china. Not cheap and very dangerous stuff. Let me know if ur interested

 

[w2x3f5]

Styrene can be reduced with zinc and hydrochloric acid in one reaction. this reaction only works for styrenes.

 

[Sonnettales]

I see. Thank you for the advise. I will use it.

 

[Sonnettales]

Question for you sir since you seem to know more than I do and have been helpful. I also have palladium on carbon %10. I assume this could be a reasonable route also but I get in trouble when I assume sometimes. Instead of the zinc and hcl.

 

[Melv99]

Also, not familiar with this particular synth but I did see K2CrO4 sold on a popular home science website. Not sure if that’s what you’re looking for.

 

[chemistry.mob]

From where did you bought the 2,5-dimethoxybenzaldehyde?

 

[Sonnettales]

Hey C.M., I did not. I started with anise oil. Read my reply above. I can send you something as well if you like via proton mail or whatever anon platform

 

[chemistry.mob]

Anise oil? it´s this a joke? LOL

 

[Sonnettales]

No joke guy. Anise oil (anethole) to anisaldehyde to o-formal-4-methoxyphenol to 4-methoxyphenol to 2-hydroxy-5-methoxybenzaldehyde to 2,5-methoxybenzaldehyde. As I mentioned above I cannot seem to attach files but if you have a protonmail account I can send you. It may be on here for all I know. I did not get it from here tho. It’s from a Dutch research report.

 

[chemistry.mob]

but you think it's profitable to do all those steps?, I don't know if you're making 2-CB for fun or to resell it.

 

[Sonnettales]

Profitable? Depends on your def of profit I guess. Most importantly? Experience. To make mistakes and learn. This stuff takes a lot of everything. Money. Knowledge. Experience. Time. Energy. It’s almost always fun for me. Maybe one day profit. But its like you said…where can you get 2,5 bnzldyd? Someone’s gotta make it thats not corporate. I’m not making enough to sell rn but maybe one day. After doing this for a couple years i can tell you if you’re doing it solely for profit, quit now and save yourself time and money. I’m a few credits short of a bachelor’s in biochem and I’ve barely scratched the surface on this stuff.

 

[Sonnettales]

I’m sorry man. I’m just now reading some of your posts above. I’m not sure what you’re doing here if you have no idea about chemistry. You don’t know how much 2-cb you’ll get from 100g of the beta-nitrostyrene? It’s almost always at the end of the whatever workup you’re following. There is more than one way of going about getting the final 2c-b product. None of them are easy or should be done by someone who has “no idea about chemistry”. Start with meth man. Decide if that’s something you think you can do or even want to do. Then go from there. No idea about chemistry. Sheesh guy.

 

[chemistry.mob]

I asked an organic chemistry professor if someone with no idea about chemistry could follow a recipe for a chemical synthesis and he said yes, that's why I joined this forum, I'm lost, I don't know what synthesis to start with, and I do it For profit, I can invest time and money to learn, my goal is to manufacture on a large scale and sell wholesale, but I see that this industry is very difficult, not only to do chemical synthesis, but also to obtain the necessary chemical reagents and precursors, Any recommendations on what synthesis to do? thank you!!

 

[nujrc]

Wut. If you do it solely for profit, why would you even want to bother with 2c series... Not addictive, niche drugs. You will have better profit by growing weed.

 

[mocnykutas]

(PDF) 2C-B Synthesis - IceCool - DOKUMEN.TIPS

2 C- B Starting from 2,5-dimethoxybenzaldehyde. First off all the coresponding nitrostyrene needs to be made. 2,5-Dimethoxynitrostyrene. 5,019g 2,5-dimethoxybenzaldehyde…

www.google.com

 

[Sonnettales]

Does anyone have a good nitromethane supplier in the US that does not report? I’ve been extracting from racing fuel but this is getting tedious. All the vendors in the ads section I’ve been in touch with are outside the US.

 

[Melv99]

I found one that sells a bunch of different fuels and claims to have 100% NitroM. Haven’t ordered yet and seems semi legit. But who knows. Guess only one way to find out.

 

[btcboss2022]

I have a doubt over the last step of 2CB synth. It says "The reaction mixture was allowed to return to room temperature, filtered, and the solids washed sparingly with cold acetic acid" until I know acetic acid becomes solid at 16-17C so what means cold acetic acid exactly?
Thanks.

 

[G.Patton]

Hi. I'm assuming that the cold acid means room temperature because there is an explanation that the reaction releases heat.

 

[nujrc]

I understand that remaining elemental bromine is going to evaporate in the air from product, just like any solvent, so there won't be any reasonable amount left with time. Making HCL without drying HBr - good luck to get more pure product, because you may have to deal with bromine salts in bromine/GAA solution, and bromine itself.

 

[w2x3f5]

I don’t see any problems to beat the remains of bromine with thiosulfate, then bring the ph to an alkaline medium and collect the oil with a solvent.