One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[aa1178251182]

No idea what went wrong, no testing equipment. The resulting amphetamine phosphate has no effect at all.

 

[chicaloca]

I have the same problem. I do the reaction and work up but I don't think the salt is amphetamine or if it is so it's a very very poor quality! What I should try to do for improving?

 

[Hank Schrader]

Make sure you have phenylnitropropene and not nitrostyrene. Perhaps you were sold an analogue, and you received phenylethylamine.

 

[diogenes]

What is the best way to check whether the nitroethane I used to make p2np has been replaced or diluted with nitromethane? I have collected the basic physical properties of both reagents and products and to me the boiling point of the nitro compound seems the most logical. Melting points of the products are very close. The problem is if the BP comes up in between the n.ethane and n.methane boiling point, then it must be a pain to separate them by fractional distillation.

The other value could be the density which is also quite different. Experts please add your opinion what is the easiest best way to ensure we are using the right reagents.

 

[G.Patton]

Hello. Nitromethane and nitroethane have different b.p. 101 and 114 °C respectively. You can check it and carry out fractional distillation. Take it into account that these substances quite toxic and explosive. So far as nitrostyrene and P2NP concerned, just use precise melting point apparatus. It is better to compare known pure P2NP with synthesized new P2NP in one apparatus to check difference. Also, carry out several measurements in order to exclude errors. Count average mp for each sample.

 

[diogenes]

Thank you Patton. I don`t have any suspicion that my nitroethane is not pure, but having read some comments, I thought it would be better to check, so I will start with the boiling point of my nitro and if it boils over 110C then I will rest assured. It is good to know what to do and check anyway, before putting in a lot of work and finding that the end-product is ineffective .

 

[chicaloca]

Hello, After the reaction I quench with dilute HCl and distill IPA off to 100°C but the next day when I come to separate the phases the flask don't stir. Theres a hue in the flask. Here is pics can someone help me to understand and telling what options I have thx

 

[WinterDust]

Hi,

First of all, where in the synthesis does it say that you should use HCL? Hint: Nowhere, so don't.

Second, since you distill in 100c I assume you do open distillation, don't do this, use vacuum distillation instead.

Try again and respost results.

Best regards

 

[chicaloca]

Okay I done it like in the OP and the phase separate after reaction and adding NaOH. So I extract the aquaous phase with IPA but in the sep funnel there is no clear separation of phases! What can I do now?

 

[UWe9o12jkied91d]

More hydroxide.
You should use a non polar such as toluene or something for extraction of the remains, even if ipa works

 

[chicaloca]

Okay Im gonna add 25% NaOH and after what should i do? Extract with DCM?
I have some

 

[chicaloca]

Okay I've add 25% NaOH but I don't think the bug came from NaOH because for phase separation it's all right... The problem occurs just after; when I want to extract the aquaus phase anyway, ... I add DCM but even with a NP like DCM there is NO CLEAR phases separation!,

 

[chicaloca]

Okay I've add 25% NaOH but I don't think the bug came from NaOH because for phase separation it's all right... The problem occurs just after; when I want to extract the aquaus phase anyway, ... I add DCM but even with a NP like DCM there is NO CLEAR phases separation!,

 

[WinterDust]

Show us a picture of how it looks...

 

[UWe9o12jkied91d]

Maybe you are not aware dcm sinks?

 

[chicaloca]

the amine should be in the upper top phase because DCM is more dense than water or IPA... but should I evaporate or steam distill?
What I do not understand is that the first DCM extract was made with 30ml DCM but the upper phase looks like more than 30ml (maybe some IPA in there?)

 

[chicaloca]

I should say down phase

 

[chicaloca]

also asure it's not a 3 phases extraction
*$*

 

[chicaloca]

I finally get some sulfate but it's not amphetamine because
I know the speed from NL what did I do wrong bosss?

 

[UWe9o12jkied91d]

First of all ipa cant be separate from dcm in a water, dcm, ipa mix.In this case the dcm and ipa will always be sepaeate from water at or around Rt.Second of all if something is more dense than water it means it will SINK, not float.DCM has 2 big Cl bois which are heavy af.
If you are confused about which is the organic layer you can drip a few drops of water and see where they go, if they fall down trough the top layer into the second layer then clearly top layer is organic

as far as effects produced by leuckart method material it can be said it is indeed different because of the residual n-formylamphetamine, which is always present to some extent in goods obtained by this route.

 

[chicaloca]

So I decante the phases and now all I have to do is waiting for DCM evap? Should I use a gentle boil? or let evap at RT?

 

[proto311]

For testing purposes I would like to compare 2 results, the first one would be amphetamine sulfate friendly for the nose, and the second one, one of those products that burns, would it make 5.5 ph and 6 a big difference in the final result? controling the ph while adding the acid to the amphetamine base, or how else can I change the ph of the final product?

 

[chicaloca]

I do the reaction and work up but I don't think the salt is amphetamine or if it is so it's a very very poor quality! What I should try to do for improving?