1-Phenyl-2-propanone (P2P) Leuckart amination to amphetamine and methamphetamine. Smale scale.

G.Patton

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Do you use reflux condenser and fume hood?
 

TheNut22

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G.Patton: Sir, can I use ethyl acetate instead of DCM in amphetamine synthesis? Or, should I use xylene instead? I mean when I have done the hydrolysis.
 

G.Patton

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Please, look through the dedicated topic and ask there. Not here.
 

Hank Schrader

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I will share the table with you.
Khi3lZJupI
 

OrgUnikum

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Maybe it is just fair to add that temperatures over 180 °C like the named 200 and 210 °C for sure completely destroy P2P and even the Formamide, the resulting vapors and gases are highly toxic. Vent everything coming from top of the condenser outsides! Seriously!
Keep it below 180, better below 175°C and calibrate the Infrared thermometer to the flask/setting you use or you will never exactly know how hot it is.

Good luck
 
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Acab1312

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The corresponding paper for isomeric separation
 

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OrgUnikum

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And as a free service from yours truly, the ratios for P2P:

Formamide 50 ml 1,5 mol
formic acid 56 ml 1,5 mol
P2P 66 ml 0,5 mol
 
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TheNut22

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Again, I really don't understand this. I never will. Why people want to synthesize amphetamines, and fail, even when someone gives right molar ratios, and then they complain that they've done everything as the procedure said, and failed again and again. Even when the right molar ratios are given, there is so much that you have to know. Or sometimes even very little, but that little bit of info is mostly crucial info to make things work. Like how many times excess one on those reagents in right molar ratio MUST BE in the reaction flask to make things work. If you are to lazy to read even one straight to the point good cook book, or you're just not enough interested to find and read even one amphetamine cook book, why you don't just buy the compound? In these forums, I see this kind of people here, that I've never seen so much, anywhere. Yes, it is very good to teach a little and give good advise, and I'm not Einstein myself, but I've studied all of my reactions from internet. Forum syntheses, read bunch of books and patents, reactions on different sites. Downloaded many basic organic chem books etc. I was bad in chemistry at school, because the school itself didn't interest me. At all. But when I started learning chemistry about 8 years ago, I'm hooked into trying new syntheses, not the drugs anymore. But this is just me, everyone is different, but sometimes I'm so annoyed with this, that I must say something. And peace out! I'm sorry for the long text.

P.S This text was not to you OrgUnikum, but .. you know, those in text.

TheNut.
 

TheNut22

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It seems I was a bit too much tired, regarding my last long post! :)
 

edy's

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Respect,not intyerly my idea,but still
 

OrgUnikum

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some people want to make drugs and some want to make money, thats the main difference. I can accept both approaches as long quality is not compromised. Sadly with both approaches it usually is and that is when I am out, I am not delkivering the fastest cheapest way to something what can be sold as drug to the usual retarded drug user.
Sorry.
Quality is much much harder then just cooking something up what has a bang of a kind.
First you just try to get a usable result.
Then you try to get it every time.
Then you start to go for better yields
And already when you have a usable result you invest a good part of it to hone your workup/purification skills. Be aware that this is a hard path in the beginning so only ever use a part of what you have for this as more often then not stuff just vanishes somehow into thin air and shitloads of solvents. Do not try to recover, its not worth it. Use only a part and laugh it off and try again. Makes more sense.
good luck!
 

TheNut22

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Yes, I have noticed, many times, that I buy many solvents, and I use them to get nothing. And again, and again. But this is so interesting that I never give up!
 

TheNut22

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You didn't get what I was saying, and I know, because I didn't get it now what I wrote... :) I was refering to those who are lazy and want to get spoon feed the right molar ratios and all that etc... ... and don't bother to read any books or texts about making compound. That is fustrating to me.
 

TheNut22

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Now, when I'm done with the heating (amphetamine), I'm doing the formyl hydrogenation with a base, so do I still put H2O2 (30%) first in the last reaction steps? What is the role of H2O2 in here?
 

TheNut22

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Well, I searched the info myself. The role of H2O2 is pretty important, considering the yields.. H2O2 is an oxidizer, but regarding to it's molecular form, I've always thought it can easily act also as reducing agent. Pretty facinating compound!
 
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TheNut22

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But I am also still skeptic myself, because I got this info on H2O2 use from AI-robot chemistry assistant, and that is the worst place to get any info regarding chemistry. I have also noticed that no one is using H2O2 at nowhere in these types of syntheses. So, when I'm now in the same place in this synthesis, I think I'll use just pure water, if someone with some knowledge could enlighten me with this. So, should I make 30% H2O2 or use just pure water at this stage?
 

edy's

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Can i just double the amount of h2o2 if my peroxide is just over 15 +%,its a bitch finding stronger in my place,ore maby some other compound to substitute?
 
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TheNut22

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One time I made around 25% H2O2 from my 12% H2O2 (wrong calculations), and it still worked for my peracetic acid!
 

TheNut22

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edy's: You can calculate how much you have to evaporate from that 15% H2O2 to make 35%, and then you can make good peracid. This was the first time I got from 40 g of MPB ---> 35,60 g of acetoxyphenylpropene. So, wow. And I made 30% H2O2 from 12% H2O2 to calculate how much water I have to remove with careful evaporation, and the peracid worked this well! But to be exact, I will put the peracid in side to 3 to 4 days with H2SO4 catalyst to make it work.
 

TheNut22

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I made my stonger hydrogen peroxides from 12% H2O2. I just carefully evaporated water from it.
I asked calculations from AI-robot assistant in chemistry. It is good at calculations, but don't expect to get right answers
from halogenations or the like ...
 
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loadingST

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I still havent tried the reaction but with good hydrolisis with KOH and then with HCL it shoud give high yield, and im afraid working with h2o2 to dont form any explosive peroxides and upon destilation to dont explode
 

TheNut22

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If it is done very carefully, and properly (not boiling, like some do), and without any distillation (I am also worried about those peroxides / explosions), I've made 35% H2O2, (it will whiten your fingers with little spilled drops), to make really working peracetic acid with my own made H2SO4-catalyst (about 75%). I keep the solution 3-4 days in my closet, and it's ready for use.
 
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