Need help convert bmk 5449-12-7 to free base A-oil

melk

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Sorry but I can't find the ratio of hydrochloric acid anywhere here in this Synthesis
 

UWe9o12jkied91d

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1. A solution of 1-phenyl-2-propanone(0,827 g, 6.2 mmol)


4. The oil was dissolved in a solution of methanol (5 ml) and 15% HCl (5 ml) and stirred at reflux for 2 h.

Account for error and we've found ourselves a ratio
 

melk

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What was the total amount of N-formylamphetamine ?
I need to know this for my calculation off HCI and methanol
 

melk

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If the amount from N-formylamphetamine is 500 ML, is it correct to add 75 ML HCI and 75 ML isopropanol alcohol ?
 

UWe9o12jkied91d

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It is not my procedure, from a thread by sir william.Having an exact number wold be ideal, but the point is HCl is used in excess, for example the paper below uses 10ml of HCl of unspecified conc. (or im blind or stupid) for 1 gram of product to be hydrolized.
https://patentimages.storage.googleapis.com/83/bb/4d/9cd8b0724ca65a/US20130046111A1.pdf
 

melk

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So many versions of this last step have been posted that searching for the right method here on breaking bad is like playing the lottery.

Uncle fester posted a clear answer, but that is not for amphetamines but meth
he only adds HCI and not HCI + Alcohol like I read here on this page.
He says if N-formylamphetamine is 500 ML than add 1 liter HCI and reflux 1 hour
but again this info is for meth, so I still have no answer.
 

Castlebar

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Thanks fol keeping me in the loop aswell
appreciated
 

Saul

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this topic is completely stuck.
no more useful answers are coming up.
 

Castlebar

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Has any asked sir William about the answer ? And thanks for reply
 

melk

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.
I even opened a ticket yesterday with this question and then I get an existing link in response where the answer is really not written. they are specialists and they are super helpful to some .
my answer is enough with 6 carackters total text
but unfortunately no one knows the answer or does not want to give it
 
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UWe9o12jkied91d

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It doesn't really matter tbh, as long as you have enough to hydrolize all the nfa a large excess dosen't seem to hurt.If literature reports good results with ratios of 5 to 1 twice, 10 to 1 once and this procedure reports around 1 to 2.5 roughly.So we can draw the conclusion anything between 2.5/100 to 10/100 works fine by my reasoning.
I think I explained pretty clearly and accurately, if any expert wants to peer review me I invite all corrections ofcourse.
 

melk

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I wouldn't need a forum if I was experimenting blindly. the amount is extremely important. also because we use HCI 30%. there's quite a bit of water in there already.
By the way, this is the last step so if you use too much, that a-oil is worth nothing.
or are there two layers added to this step ?
If so then it can't hurt to use too much.

are there after the reaction HCI + reflux 2 hour also 2 Layers ?
 

Castlebar

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Hi guys I will be attempting to turn the p2p into pn2p using described methods available on here if anyone has anything to add information wise it is appreciated I know there are many knowledgeable people on this forum and guys your knowledge and wisdom is appreciated so please feel free any of you to offer your direction many thanks
 

Saul

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hello, my friend,

I am close to final I don't rush things don't like that I take my time
and only goes to the next level if I am 100% sure it is right.
But I promise when I am there, I write down in detail every step I did to the end.
in my group breaking bad europe. ( for al sponsor members ) to support the forum
 
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Castlebar

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Hello Saul thanks for reply yeah I been going steady with this to just managed to get a improved yield from the glicidiate and conversion into dark rich oil bmk my end product will hopefully produce anphetamine sulfate and great I look forward to hearing how you get on fingers crossed 🤞 it goes well
 

Kslzlxczkaoxl

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Posting from a burner since I can’t log my main now.
I mean you’ve got a huge margin 2.5/100-10/100 so I doubt you can screw up too too bad.It dosen’t matter within reason ofcourse, but start conservatively and see what works and what dosen’t, it’s not blind if you have a generous interval.
And yes, after the extracting of n-formyl by distillation or solvent you will have 1 layer in the flask, and after hcl you will naturally have 2 layers since there is water in the acidic solution.After hydrolysis you then again separate the 2 layers extracting your freebase a few times with a non polar solvent or distillation.

Good on you, sir.Praxis, action is the only way to master a reaction, regardless of theory or disscussion over small details.Keep us posted.
 
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Castlebar

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Thanks for your reply I'm working steadily at this to try and reach the end result and will share my findings also at the end guys all information knowledge and feed back from you all is appreciated this forum is fantastic in that way have a good day all of you
 

melk

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so just an update on the situation.
so i had 400ml of N-Formylamphetamine and I added 800ml of hydrochloric acid and boiled reflux for 2 hours.
the color is horribly very dark brown. now I'm curious if I'm going to see two layers since the color is so fuckt up. I really hope so. then I just need to get the ph up and for this I use naoh mix with water. now i'm going to let everything cool down
 

melk

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https://bbgate.com/attachments/snbp7j6cis-jpg.6792/?hash=3ae4cd3bf8d82f5114d358d291f71215

this is how it looks after the HCI room temp
 

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