Aminación Leuckart de 1-fenil-2-propanona (P2P) a anfetamina y metanfetamina. Escala pequeña.

[Selassi]

Swim recibió una pregunta sobre una variación diferente de este método:

Después del primer paso (ebullición con fórmico y formamida), ahora vuelven a hervir la fase orgánica con agua y NaOH en lugar del reflujo con HCl.

¿Alguien me puede explicar la métrica de este segundo paso diferente? Swim nunca lo ha hecho de esta manera, pero parece ahorrar mucho tiempo en contraste con el método oldschool con reflujo HCl.

¿Qué concentración de sosa cáustica/agua y qué cantidad se introduce en el reactor por L de producto?
¿Cuánto tiempo debe hervir esta mezcla de reacción y a qué temperatura?

 

[waltjr5858]

You can do hydrolysis with a base or an acid...

 

[Curiousonion]

¿Por qué un rendimiento tan bajo para esto, alguien tiene un método de mayor rendimiento para la metanfetamina?

 

[Chemdog010297]

Red p, maybe aluminum

 

[Saul]

eso no es correcto información errónea ese tipo de tesis cometen grandes errores

el carbonato de amonio nunca se utiliza directamente con p2p.
Primero se fabrica el formiato de amonio.
El formiato de amonio se hace fácilmente a través de carbonato de amonio y ácido fórmico. Titule
a un buen pH de 7 y eliminar el agua.
Sólo entonces se puede utilizar con p2p

 

[waltjr5858]

Yes ammonium carbonate can completely be used in this reaction directly it's actually a very popular method in many countries and makes ammonium formate in situ.... if you're not 100% sure what you're saying on here don't

 

[G.Patton]

¿Utiliza condensador de reflujo y campana extractora?

 

[waltjr5858]

In a write up that most people are reading to do this leuckart with formamide and p2p specifically... what is the purpose of a 15 min reflux with 30% h2O2 with the reaction mixture after you have already done the first reflux with formamide and p2p. Does it clean up or oxidize something? I mean this is prior to the hydrolysis. I just can't think of what it would do. I mean most people do it without it but it was obviously added for a reason in a actual professional write-up.

 

[G.Patton]

Sorry, but I don't clearly understand about what "15 mix reflux" are you talking about? Can you be more precise. Refer to a step number.

 

[waltjr5858]

It's not on these instructions. When making amphetamine after the first 24 hour reflux on a different set of instructions they would reflux for 15 minutes with 30% hydrogen peroxide and then go on with hydrolysis. What was the point of the peroxide?

 

[G.Patton]

I have no Idea about what "different set of instructions" are you talking and hence can't answer your question.

 

[waltjr5858]

Ok... but in general then what would happen to the resulting solution if spun up with 30% peroxide?

 

[William Dampier]

El uso de una cantidad adicional de agua en la reacción de Leuckart puede aumentar el rendimiento. Quien lo haya hecho, puede escribir sobre ello aquí.

 

[TheNut22]

En Leuckart, hay que asegurarse de que no haya nada de agua.

 

[southcost]

But we have a 12% water at least in our formic acid, isn't it?

 

[TheNut22]

Hice mis peróxidos de hidrógeno más fuertes a partir de H2O2 al 12%. Evaporé cuidadosamente el agua que contenía.
Le pedí cálculos al asistente robot de química. Es bueno en los cálculos, pero no esperes obtener respuestas correctas...
de halogenaciones o similares ...

 

[loadingST]

Todavía no he probado la reacción pero con una buena hidrólisis con KOH y luego con HCL debería dar un alto rendimiento, y me temo que trabajando con h2o2 para no formar peróxidos explosivos y al destilar para no explotar.

 

[William Dampier]

Yes, it is better to exclude peroxide.

 

[YenaneY]

This questions are mainly regarding the actual chemistry behind the synthesis...
Why does one for the formation of the amine from the intermediate need H2O2 and HCl in the synthesis of amphetamine but only HCl in the synthesis of methamphetamine?

 

[William Dampier]

In fact, there is no need to use peroxide.

 

[waltjr5858]

But what was the purpose of the peroxide in the first place I believe he's asking

 

[waltjr5858]

I saw the same thing and nobody has an answer for it but it was done by actual professional chemist.... not clandestine hackers so id say its there for a reason but it will work without it. Probably to kill off so.e kind of side product or something.

 

[YenaneY]

I think it really is because the hydrogen peroxide helps promote the reaction, but the reaction of deformylation is generally easier on tertiary amines compared with secondary ones, which is why it happens more readily if N-methylformamide is used for methamphetamine.

 

[Pinkbay]

sir, In step 3, is heating required?

 

[rampage]

can you replace n-methylformamide with dimethylformamide?

 

[waltjr5858]

I don't think so