aa1178251182

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No idea what went wrong, no testing equipment. The resulting amphetamine phosphate has no effect at all.
 

G.Patton

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Hank Schrader

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No idea what went wrong, no testing equipment. The resulting amphetamine phosphate has no effect at all.
aa1178251182Make sure you have phenylnitropropene and not nitrostyrene. Perhaps you were sold an analogue, and you received phenylethylamine.
 
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aa1178251182

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Make sure you have phenylnitropropene and not nitrostyrene. Perhaps you were sold an analogue, and you received phenylethylamine.
Hank SchraderI request to purchase CAS705-60-2. I bought two barrels, which have changed color after being stored for a long time, and the discolored raw materials were recrystallized with absolute ethanol to restore their original appearance. The merchant clearly stated that they are CAS705-60-2. I experimented with LAH and got the same product that didn't work. I don't know where the problem is.
 

Hank Schrader

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I request to purchase CAS705-60-2. I bought two barrels, which have changed color after being stored for a long time, and the discolored raw materials were recrystallized with absolute ethanol to restore their original appearance. The merchant clearly stated that they are CAS705-60-2. I experimented with LAH and got the same product that didn't work. I don't know where the problem is.
aa1178251182Most likely you are dealing with nitrostyrene, which is obtained from nitromethane with benzaldehyde. This often happens in the precursor market. Also, due to the problem of getting nitroethane, often styrene is mixed in and you end up with a mixture of amphetamine and phenylethylamine.
 

G.Patton

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I request to purchase CAS705-60-2. I bought two barrels, which have changed color after being stored for a long time, and the discolored raw materials were recrystallized with absolute ethanol to restore their original appearance. The merchant clearly stated that they are CAS705-60-2. I experimented with LAH and got the same product that didn't work. I don't know where the problem is.
aa1178251182As I told you before, you can check the melting point of your reagent and product and you'll figure out was it p2np or nitrostyrene as Hank said.
 

KokosDreams

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After evaporating the IPA off the freebas/IPA solution, the compound has turned into a thicker mass than expected when we removed it from the rotovap (picture attached).

Our plan was to do a steam distillation (1:1 water ratio) and two DCM extractions after.

Unfortunately, after combining the extracted aeqeous layer with the organic layer + filtering + drying both, the bottom of the flask has turned into a gele like it happened to many others on this forum after letting it rest over night at around 7-9 °C.
Our assumption to this is that either the drying agent Sodium sulphate or leftover sodium hydroxide from the NaOH solution has remained in the solution throughout the filtering process which now caused the oil to become thicker than expected after evaporating the IPA.

My question is, should we still continue with a steam distillation + dcm extraction now?
Or are there other options to reclaim the fluid state of the freebase?

Cincerly,

Koko
 

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UWe9o12jkied91d

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What did you use to dry? Calcium salt i’m guessing?
@KokosDreams

ah sodium sulphate, I’m blind.Did you buy it anhydrous or dry yourself?
Mass gells up with calcium salts or in combination with water mostly (freebase + water = gel)
 

KokosDreams

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What did you use to dry? Calcium salt i’m guessing?
@KokosDreams

ah sodium sulphate, I’m blind.Did you buy it anhydrous or dry yourself?
Mass gells up with calcium salts or in combination with water mostly (freebase + water = gel)
UWe9o12jkied91dWe bought it anhydrous.

After a few chats with some people here we have now decided to prepare a 10ml sample from the compound and mix it with 100ml of d2h2O to then extract it with 16ml DCM.
Attached you can see the compound + water solution aswell as how it looked after adding dcm.

The experiment would now be to prepare another 10ml sample of the compound, carry out a steam distillation + dcm extraction to see if we can get the result to crystalize with acetone, methanol and sulphuric acid

I will also attach a picture of another sample I put aside from the organic & aeqeous layer
 

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UWe9o12jkied91d

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We bought it anhydrous.

After a few chats with some people here we have now decided to prepare a 10ml sample from the compound and mix it with 100ml of d2h2O to then extract it with 16ml DCM.
Attached you can see the compound + water solution aswell as how it looked after adding dcm.

The experiment would now be to prepare another 10ml sample of the compound, carry out a steam distillation + dcm extraction to see if we can get the result to crystalize with acetone, methanol and sulphuric acid

I will also attach a picture of another sample I put aside from the organic & aeqeous layer
KokosDreamsOh I see now , I would just distill that, it's just an emulsion, this is how it's gonna come over in your dean stark or wherver you are collecting first few ml till steam picks up.Also you're way off on the ratios, it will take like a whole liter of agua to distill over MAYBE 100 of base depending on steam temp, source of steam etc.
I suggest external source of steam, maybe immersion heater in a flask + heating of the base container.
 

KokosDreams

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Oh I see now , I would just distill that, it's just an emulsion, this is how it's gonna come over in your dean stark or wherver you are collecting first few ml till steam picks up.Also you're way off on the ratios, it will take like a whole liter of agua to distill over MAYBE 100 of base depending on steam temp, source of steam etc.
I suggest external source of steam, maybe immersion heater in a flask + heating of the base container.
UWe9o12jkied91dLet's continue in DMs
 

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Fellas is it possible to run this with NaBH3CN? Thank you
 

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Hello
after the batch 1kg p2np we have about 10l of diluted ipa/amphetamine, why do we have to add more ipa/acetone to this before we drip in sulfuric acid when there is already enough ipa in it.

when we have pure amphetamine base, we dilute this with amf/ipa 1:2 or 1:3 before adding sulfuric acid...

and is it possible to run the synth with methanol/h20 instead of ipa..

Thanks :)
 

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Hello
after the batch 1kg p2np we have about 10l of diluted ipa/amphetamine, why do we have to add more ipa/acetone to this before we drip in sulfuric acid when there is already enough ipa in it.

when we have pure amphetamine base, we dilute this with amf/ipa 1:2 or 1:3 before adding sulfuric acid...

and is it possible to run the synth with methanol/h20 instead of ipa..

Thanks :)
SwesweWondering this myself. Unless I'm mistaken or missing something.. We evap IPA to leave FB then add IPA/Acetone. Can't we go straight to Acetone/Sulfuric since it's already in IPA?
 

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Wondering this myself. Unless I'm mistaken or missing something.. We evap IPA to leave FB then add IPA/Acetone. Can't we go straight to Acetone/Sulfuric since it's already in IPA?
Marvynyes, it is fine to add sulfuric acid directly to the ipa/amf base, it was a mistake on my part, I thought they added ipa and acetone, acetone is to clean the product I guess, but it works well without acetone included.
 

UWe9o12jkied91d

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Wondering this myself. Unless I'm mistaken or missing something.. We evap IPA to leave FB then add IPA/Acetone. Can't we go straight to Acetone/Sulfuric since it's already in IPA?
MarvynYou can add conc. sulphuric but its always a good idea to dillute it with some acetone.Dropping it in conc. leads to local over-acidification, where regardless of basic medium a portion of your product will be irreversibly destroyed.
 

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Hello
after the batch 1kg p2np we have about 10l of diluted ipa/amphetamine, why do we have to add more ipa/acetone to this before we drip in sulfuric acid when there is already enough ipa in it.

when we have pure amphetamine base, we dilute this with amf/ipa 1:2 or 1:3 before adding sulfuric acid...

and is it possible to run the synth with methanol/h20 instead of ipa..

Thanks :)
Sweswe
and is it possible to run the synth with methanol/h20 instead of ipa..
Yes, it is possible. You have to use pure alcohols.
 
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