One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)
- Thread starter GhostChemist
- Start date
Hi,
I have just done this synthesis and the yield is 60%+ (some acetone still in the freezer), which is not bad considering that at some point the reaction mass spillt out (overheated and started to expand). I quickly cooled it and then kept a reflux condenser on top for the rest of the reaction (the original description does not mention this). There is some delay in the heat increase following the addition of a portion of the P2NP, which needs to be considered, I added a further portion too quickly. A cold bath is handy. The endproduct is very efficient in terms of bio-test, I am doing an acid-base extraction to see whether there are other chemicals is the endproduct as well. There is a slight, distinct smell, which I identify as close to the smell of Cu perhaps?, which lingers despite 5X Acetone wash and having a very white, pure looking product.
I was wondering if there is anyone here, who could write out the exact reaction what is happening in this synthesis. The role of CuCl2 is not clear to me and also how the H atoms move etc. It would be very useful to have the reaction explained in a bit more detail. Apologies, if this has already mentioned, I have seen most of this thread, but haven`t had the chance to catch up lately. Thank you
I have just done this synthesis and the yield is 60%+ (some acetone still in the freezer), which is not bad considering that at some point the reaction mass spillt out (overheated and started to expand). I quickly cooled it and then kept a reflux condenser on top for the rest of the reaction (the original description does not mention this). There is some delay in the heat increase following the addition of a portion of the P2NP, which needs to be considered, I added a further portion too quickly. A cold bath is handy. The endproduct is very efficient in terms of bio-test, I am doing an acid-base extraction to see whether there are other chemicals is the endproduct as well. There is a slight, distinct smell, which I identify as close to the smell of Cu perhaps?, which lingers despite 5X Acetone wash and having a very white, pure looking product.
I was wondering if there is anyone here, who could write out the exact reaction what is happening in this synthesis. The role of CuCl2 is not clear to me and also how the H atoms move etc. It would be very useful to have the reaction explained in a bit more detail. Apologies, if this has already mentioned, I have seen most of this thread, but haven`t had the chance to catch up lately. Thank you
- By mile123
Hello!
What reflux condenser do you recommend, is Friedrichs really worth double the price compared to Graham?
www.laborxing.com
I read here that @OrgUnikum recommends Friedrichs.
I'm thinking about adding reflux condenser at 3. step
because of suggestion below
and possible h2 production safety reasons
Br,
Mile
What reflux condenser do you recommend, is Friedrichs really worth double the price compared to Graham?
Condensers
Laborxing.com, one stop online shop for lab glasses, lab equipment and chemicals.
www.laborxing.com
I read here that @OrgUnikum recommends Friedrichs.
I'm thinking about adding reflux condenser at 3. step
because of suggestion below
and possible h2 production safety reasons
Br,
Mile
I forgot to mention in my post that I heavily scaled down the synthesis, using only 25g of P2NP. I simply divided everyting by 1000/25=40 and used a 2l flask. Although the amount was less than half of the flask I still managed to spill some so I would suggest using a reflux by default to prevent this or just keep in mind that following the addition of a portion of P2NP there is a time-lag until it starts reacting so the addition should be real slow and gradual. This is definitely what I`m going to use next time. The other change I did was to reduce the amount of solvent in the end (not until only oil was left) and then precipitate by IPA-Sulphuric acid (10-1) until Ph 6-7.
Obtained yield from 100g P2NP as starting material was 78g pure white dried sulfate
Used was IPA/water in 2:1 ratio like in original synthesis (1200ml IPA / 600ml Water)
150g NaBH4, added in 2 portions, first portion 100g at the start mixed with ipa and water
Then after all the p2np has been added (when adding p2np use cold water for cooling the vessel)
Then added 50g NaBH4 again to vessel, and proceeded to heat the mixture to 50 degrees
and when the reaction was hot in one portion added 30g of CuCL2 (CuCl2 was dissolved in 100ml IPA / 50ml water)
Addition produced volcano style eruption which blew a bit of CuCl2 out of vessel - but not a problem
After this step, reaction was heated to a boil for good 45 minutes, after it was basified with NaOH and separated the top layer
Which was IPA with freebase
Water cooled condenser on vessel has been used from start to finish, otherwise you will lose too much solvent
And I also can confirm the smell you @diogenes are experiencing, the same weird smell after Cu - even after numerous IPA cleanings of product
Maybe after few days outside it will subside
Nevertheless this reaction is one of the most cleanest and simplest reactions ever done in one pot
Used was IPA/water in 2:1 ratio like in original synthesis (1200ml IPA / 600ml Water)
150g NaBH4, added in 2 portions, first portion 100g at the start mixed with ipa and water
Then after all the p2np has been added (when adding p2np use cold water for cooling the vessel)
Then added 50g NaBH4 again to vessel, and proceeded to heat the mixture to 50 degrees
and when the reaction was hot in one portion added 30g of CuCL2 (CuCl2 was dissolved in 100ml IPA / 50ml water)
Addition produced volcano style eruption which blew a bit of CuCl2 out of vessel - but not a problem
After this step, reaction was heated to a boil for good 45 minutes, after it was basified with NaOH and separated the top layer
Which was IPA with freebase
Water cooled condenser on vessel has been used from start to finish, otherwise you will lose too much solvent
And I also can confirm the smell you @diogenes are experiencing, the same weird smell after Cu - even after numerous IPA cleanings of product
Maybe after few days outside it will subside
Nevertheless this reaction is one of the most cleanest and simplest reactions ever done in one pot
Why did you add so much CuCl2? I was thinking that the weird smell might be due to impurities in my CuCl2 (which I prepared from some copper pipes), but if you had the same it means there might be some Cu or Cu related impurities in the product. By the way, I did an acid base extraction on some portion of the yield and the smell completely disappeared.
Uncle Lee, I have just realised that you said some very important things which I don`t fully understand. What do you mean by nanoparticles? In general I don`t understand the role of CuCl2 in the reaction, can you please explain this and also the nanoparticles part? Apologies for the delayed reaction to your post.
A NaOH (8 liters 25%) water solution of is added to the reaction mixture and layers are separated.
I have sodium hydroxide granules, how do I make them 25% solution ?
I have sodium hydroxide granules, how do I make them 25% solution ?
You can find plenty of videos on youtube. Basically find some pure copper (e.g. wires etc.) then add some HCl and H2O2. If your hydrogen peroxide is strong then add it very carefully as the reaction can be quite stormy.
1 liter of distilled water + 250g of NaOH. It refers to the weight percentage and 1l of water is 1000g.
1 liter of distilled water + 250g of NaOH. It refers to the weight percentage and 1l of water is 1000g.
20% NaOH (W/V), means 20 grams of NaOH solids, dissolved in distilled water until you have 100mL of aqueous solution. Do this in beaker slowly, and drip water until it reaches exactly 100 mL mark. 20% NaOH(W/W) means 20 grams of NaOH solids plus 80 grams of distilled water, making up 100 grams of solution.
So, I started my first synthesis today, did not go very well.
The reaction at higher volumes is VERY exothermic (200g P2nP) and just as previous poster stated, it's a very delayed reaction.
I used a 10l roundbottomflask with a 400mm cooler, unfortunetly I added too much P2nP at once (100G) and the cooler broke of accidently, so I had a 1m (3foot) volcano in my house
..
Well, spent 2 hours cleaning everything when everything calmed down and I ventilated the whole room.
So lesson, there is a delayed reaction when adding the P2nP so poor very gently and wait, secondly be vary of a good chilled cooler connected.
I'll do my second attempt tomorrow or the day after.
I'll keep people posted, best regards.
The reaction at higher volumes is VERY exothermic (200g P2nP) and just as previous poster stated, it's a very delayed reaction.
I used a 10l roundbottomflask with a 400mm cooler, unfortunetly I added too much P2nP at once (100G) and the cooler broke of accidently, so I had a 1m (3foot) volcano in my house
..Well, spent 2 hours cleaning everything when everything calmed down and I ventilated the whole room.
So lesson, there is a delayed reaction when adding the P2nP so poor very gently and wait, secondly be vary of a good chilled cooler connected.
I'll do my second attempt tomorrow or the day after.
I'll keep people posted, best regards.