Syntheses of 2C-phenylethylamines

[chemistry.mob]

Could you tell what laboratory equipment is required for the chemical synthesis of 2-CB?

 

[w2x3f5]

Could you tell what laboratory equipment is required for the chemical synthesis of 2-CB?

chemistry.mobit all depends on the way of synthesis. you need a starting point and the path you want to follow.

 

[chemistry.mob]

it all depends on the way of synthesis. you need a starting point and the path you want to follow.

w2x3f5i want to follow the chemical syntesis of 2-CB posted in this post

 

[w2x3f5]

i want to follow the chemical syntesis of 2-CB posted in this post

chemistry.mobHenry reaction, flask, reflux condenser, heated magnetic stirrer, water bath (or do it in the microwave), measuring cylinder, vacuum filter Buchner funnel and Bünsen flask and the filters themselves, heat-resistant beakers low spout
Reduction on lithium aluminum hydride is all the same, only ice and a dropping funnel will be needed to drop the styrene solution, and then we drop in ethyl acetate or ethyl alcohol in order to use up the excess lithium aluminum hydride.
Bromination is the same
scales and the like.

 

[w2x3f5]

i want to follow the chemical syntesis of 2-CB posted in this post

chemistry.moblithium aluminum hydride doesn't like jokes and likes to explode and set fire to solvents. it cannot be extinguished with water, carbon dioxide, else he not like peroxide and water in THF

 

[chemistry.mob]

lithium aluminum hydride doesn't like jokes and likes to explode and set fire to solvents. it cannot be extinguished with water, carbon dioxide, else he not like peroxide and water in THF

w2x3f5So it would be better to use a chemical reactor to prevent it from exploding and harming me? And if so, what capacity should the chemical reactor be?
Have you made 2C-B before?
thanks!

 

[w2x3f5]

So it would be better to use a chemical reactor to prevent it from exploding and harming me? And if so, what capacity should the chemical reactor be?
Have you made 2C-B before?
thanks!

chemistry.mobhow will the reactor help you? work correctly with lithium aluminum hydride, everything is as dry as possible, good cooling, the absence of peroxide impurities in the solvent.
I did it in an ordinary three-necked flask in an ice bath, sometimes with explosions and fires, in the first syntheses, then I learned =)

 

[UWe9o12jkied91d]

So it would be better to use a chemical reactor to prevent it from exploding and harming me? And if so, what capacity should the chemical reactor be?
Have you made 2C-B before?
thanks!

chemistry.mobIt would be better to just not use THF if youre asking questions like this

 

[w2x3f5]

It would be better to just not use THF if youre asking questions like this

UWe9o12jkied91dbad advice) I can already imagine how dry styrene is mixed with aluminum hydride (dioxane has the same problems of fluorine and thf)

 

[chemistry.mob]

It would be better to just not use THF if youre asking questions like this

UWe9o12jkied91dmate, I have no idea about chemistry, I'm trying to learn, but it's frustrating, too much information, I still don't know which chemical synthesis to stay with and focus on it, I'm thinking either 2-CB or MDMA, unless I changed my mind, at first I wanted to do the synthesis of LSD but I have seen that the synthesis for the manufacture of only lysergic acid, the precursor of LSD, is very complex and requires many reagents and chemical reactions.
thank you!

 

[w2x3f5]

mate, I have no idea about chemistry, I'm trying to learn, but it's frustrating, too much information, I still don't know which chemical synthesis to stay with and focus on it, I'm thinking either 2-CB or MDMA, unless I changed my mind, at first I wanted to do the synthesis of LSD but I have seen that the synthesis for the manufacture of only lysergic acid, the precursor of LSD, is very complex and requires many reagents and chemical reactions.
thank you!

chemistry.mobLAH not for beginner

 

[chemistry.mob]

how will the reactor help you? work correctly with lithium aluminum hydride, everything is as dry as possible, good cooling, the absence of peroxide impurities in the solvent.
I did it in an ordinary three-necked flask in an ice bath, sometimes with explosions and fires, in the first syntheses, then I learned =)

w2x3f5My friend, from where did you bought (CAS: 93-02-7)?

2,5-Dimethoxybenzaldehyde​

I found a seller on alibaba that supposedly sells it, but how can I make sure that is that substance when I receive it?
And what´s the difference between that and this 2,5-dimethoxy-beta-nitrostyrene?
Thank you! and sorry, but i have no idea about chemistry.

 

[w2x3f5]

My friend, from where did you bought (CAS: 93-02-7)?

2,5-Dimethoxybenzaldehyde​

I found a seller on alibaba that supposedly sells it, but how can I make sure that is that substance when I receive it?
And what´s the difference between that and this 2,5-dimethoxy-beta-nitrostyrene?
Thank you! and sorry, but i have no idea about chemistry.

chemistry.mobthe first is aldehyde, the second is nitrostyrene. the difference besides the fact that in the formula, they have different physical and chemical properties
check melting point

 

[UWe9o12jkied91d]

My friend, from where did you bought (CAS: 93-02-7)?

2,5-Dimethoxybenzaldehyde​

I found a seller on alibaba that supposedly sells it, but how can I make sure that is that substance when I receive it?
And what´s the difference between that and this 2,5-dimethoxy-beta-nitrostyrene?
Thank you! and sorry, but i have no idea about chemistry.

chemistry.mobI have both the styrene and aldehyde for sale if you are interested.

 

[chemistry.mob]

I have both the styrene and aldehyde for sale if you are interested.

UWe9o12jkied91dWhat´s the price?

 

[UWe9o12jkied91d]

What´s the price?

chemistry.mob180 euros for 100g of the styrene and 120 euros for 100g of the aldehyde

 

[chemistry.mob]

180 euros for 100g of the styrene and 120 euros for 100g of the aldehyde

UWe9o12jkied91dThe problem is that I don't know that with 100g how much 2-CB I can get

 

[UWe9o12jkied91d]

The problem is that I don't know that with 100g how much 2-CB I can get

chemistry.mobSound like a you problem

 

[chemistry.mob]

Sound like a you problem

UWe9o12jkied91dI already told you, that i have no idea about chemistry.

 

[UWe9o12jkied91d]

I already told you, that i have no idea about chemistry.

chemistry.mobAgain, sounds like a you problem

 

[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]

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.

Sonnettalesusually, 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]

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

w2x3f5Question 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]

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

SonnettalesAlso, 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]

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.

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

 

[chemistry.mob]

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.

SonnettalesI 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]

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!!

chemistry.mobWut. 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.