Amphetamine Synthesis From P2NP via SnCl2 and Zn

[Madeinkorea]

Очень интересный синтез!
У меня вопрос по части, когда мы впервые добавляем NaOH в смесь (5-й шаг), после того, как раствор NaOH был добавлен в смесь, добавляем ли мы этил-ацетат в смесь, чтобы мы могли отделить оксим от ацетона, или я что-то не так понимаю.

 

[yuiopjkl]

Да, этилацетат используется для выделения оксима из смеси

 

[Acab1312]

Could one not evaporate the ethyl acetate? To obtain the p2p oxime as a solid, recrystallize it once. The oxime is stable in storage....And if needed, hydrolyze to p2p. The process sounds familiar to me from the hive.

 

[mithyl2]

В зависимости от того, в какой точке мира вы находитесь, вы можете купить наборы для тестирования реагентов.

Наберите в гугле "наборы для тестирования реагентов".

вы имеете в виду, является ли нюхание хорошим способом тестирования продукта?

 

[TucoSalamanca.]

Нужно ли повторно экстрагировать продукт после a/b-экстракции?

 

[waltjr5858]

Never ever trust an online synthesis until you have verified that it works on a very small amount. 95% of them are all fake that are missing all kinds of steps in between or times or temperatures or whatever that will cause it to fail.

 

[NieDoswiadczony]

can ipa be used instead of acetone for p2np?

 

[waltjr5858]

At the beginning portion? Definitely not.

 

[waltjr5858]

That last picture also.... I think that's the cleanest Amp base I have ever seen post reaction.

 

[waltjr5858]

On step 4.... where it says after stirring for 20 minutes to add 4ml of HCL... I know when p2np is reduced with sncl2 you are either getting the ketoxime or the oxime... it just says add 150ml of cold water and 4ml of HCL.. and then it goes straight to the next step? Or are we waiting for that color change?

 

[michelAMPH2]

Hoe activeer ik Tin Chloride?
Als ik 30% HCI aan het azijnzuur toevoeg, hoeveel is dat dan?

 

[whitefighter]

Hi people. Can someone please write a reasonable schedule? I do not understand a few things and find that some are incomprehensible.


No. 1. Solution of P2NP in Acetone +

Add acetone and 42 g tin(II) chloride dihydrate


from when do I have to cook???

i.e. from when? at how much degree C? and how long pre-altooth?

How do I see when the reaction is ready?

 

[michelAMPH2]

How do I activate Tin Chloride?
If I add 30% HCI to the acetic acid, how much is that?

 

[waltjr5858]

You don't need to activate the tin chloride. It will react with p2np and form the ketoxime just give it an hour or so to fully finish. On the second reaction the problem is the double bond.... it will reduce the ketoxime to amine but if the double bond is still there it's useless. In order to give you the best chance at saturating the bond i would reflux with zinc and GAA for at least 4 hours or it's not going to go. These directions have eaten quite a few people's p2np so beware and try to do a smaller batch and change the second step to a 4 hour reflux....

 

[michelAMPH2]

you mean 4 hours reflux with the step hydrochloric acid and acetic acid?
or the first reaction after reacting 4 hours reflux

 

[waltjr5858]

The second part where you react zinc and glacial acetic acid. You don't need hydrochloric acid that's almost too strong. The keto oxide will reduce to the amine fairly quickly but the double bond is the reason to take it up to reflux for 4 hours. The rest of the steps up till that point just follow them.

 

[whitefighter]

yes.. at the first reaction? how long? do I have to heat it myself or just let it react?

 

[waltjr5858]

Just let them react together for like an hour... you do not need heat. The reaction will heat itself up probably to 40 to 50 Celsius and when it's completed it will come down to room temperature by itself. No heat needed

 

[whitefighter]

That's what I've done so far. Then I put 150 ml of cold water and 4 ml of 36% hydrochloric acid in a glass and slowly add it to the mixture while stirring. Then I added the sodium hydroxide solution (200 g to 200 ml of water)...now I have 3 layers, the top one is red...what should I do or did I do something wrong?

 

[whitefighter]

Extract 3 x 50 ml of ethyl acetate. Dry with anhydrous magnesium sulfate. Put 60 ml of glacial acetic acid in a beaker on a magnetic stirrer and add the previously obtained solution (oxime in ethyl acetate).

I don't understand that part?

So I should take the remaining liquid and do what with it? Wash it 3 times with ethyl acetate or what??

Dry it with anhydrous magnesium sulfate.? That means?

Lg

 

[Josetetete10]

Would this reaction work for the reduction of dimethoxy nitrostyrene?

 

[waltjr5858]

I actually got this one to work on a nitropropene. Well many things were changed for it to actually work but if you have zinc and tin ii chloride and also ammonium chloride it will work…. But not as posted

 

[LITHIUMONE]

Hi, I recently made some phenylacetone oxime, dissolved 3g in 50mL IPA and added 55g GAA.
10g of Zn dust was added, sonicated @30-40c for 2.5hrs, cooled.
Basified with 55g NaOH in 200g H2O, cooled in waterbath.

Vacuum filtered Zn, separated off IPA in sep-funnel.
Washed IPA with 25% cold NaOH 4x.
Dried IPA over 3hrs with 50g Na2SO4, filtered.

dextro-Tartaric acid (L-tartaric) dissolved in IPA and added.
Creamy white precipitate filtered, dried.
720mg of dextroamphetamine bitartrate was collected (~25%)

Attached below is pictures of NH2OH/Na2CO3/Oxime/IPA
and dextroamphetamine tartrate, along with filtrate that has slowly gone
pinkish over several days of standing with levoamphetamine in solution.

This acquired compound shows up a positive for mandelin reagent kit and after
several bio-assays I can indeed say it is amphetamine.

 

[William D.]

did u activate the zinc?