Leuckartova aminace 1-fenyl-2-propanonu (P2P) na amfetamin a metamfetamin. Směsné měřítko.

Selassi

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Plavec dostal otázku týkající se jiné varianty této metody:

Po prvním kroku (vaření s mravenčím a formamidem) se nyní místo refluxu s HCl znovu vaří organická fáze s vodou a NaOH.

Může mi někdo vysvětlit metriku tohoto odlišného druhého kroku? Swim to takto nikdy nedělal, ale zdá se, že to ušetří spoustu času na rozdíl od oldschoolové metody s refluxem HCl.

Jaká síla žíraviny/vody a kolik se jí do reaktoru přivádí na 1 l produktu?
Jak dlouho by se měla tato reakční směs vařit a při jaké teplotě?
 

Saul

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To není správné špatné informace, že diplomant dělá velké chyby

Uhličitan amonný se nikdy nepoužívá přímo s p2p.
Nejprve se vyrobí mravenčan amonný.
Formát amonný se snadno vyrobí prostřednictvím uhličitanu amonného a kyseliny mravenčí. Titrace
na pěkné pH 7 a odstraňte vodu.
Teprve potom jej lze použít s p2p.
 

waltjr5858

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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

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Používáte zpětný chladič a digestoř?
 

waltjr5858

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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.
 
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G.Patton

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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

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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

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

waltjr5858

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

William Dampier

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Použití dalšího množství vody v Leuckartově reakci může zvýšit výtěžnost. Kdo to dokázal, může o tom napsat zde.
 

TheNut22

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Ano, v Leuckartu se musíte ujistit, že tam vůbec není voda.
 

southcost

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

TheNut22

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Silnější peroxidy vodíku jsem vyrobil z 12% H2O2. Jen jsem z něj opatrně odpařil vodu.
O výpočty jsem požádal AI-robota-asistenta v chemii. Ve výpočtech je dobrý, ale nečekejte, že dostane správné odpovědi.
z halogenace nebo podobně ...
 
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loadingST

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Ještě jsem reakci nezkoušel, ale při dobré hydrolýze s KOH a pak s HCL by to mělo dát vysoký výtěžek, a obávám se, že při práci s h2o2 se nevytvoří žádné výbušné peroxidy a při destilaci nevybuchnou.
 

YenaneY

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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?
 

waltjr5858

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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

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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

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sir, In step 3, is heating required?
 

rampage

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can you replace n-methylformamide with dimethylformamide?
 
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