Hey Folks
I looked at some Threads now and found nothing about amphetamine synthesis using urushibara (Nickel chloride & zinc dust(for example)
I had read how to convert Bmk glycidate to bmk oil, good information i did not know before.
But i would like to try a way without mercury chloride/nitrate.
NaBH4/CuCl2 is one option but better in large scale. It is the same for NiCl₂?
I know, the yield should not be as good as Al/Hg, but bmk is not very expensive, i can get it for aprox 70$ per kilo, so even if yield is only 30%, it would not be so bad as it sounds.
I found this informations about that Route:
(Maybe there a some ideas how to do it better)
Dissolve 4.0g Nickel Chloride hydrate (light green crystals) in 75 ml 95% ethanol w/ mag stirring and warming to 50°C. After salt is dissolved remove stir bar and add 1ml water and 1ml conc. HCl.1 While solution at 50°C slowly add 5g regular Reynolds wrap torn up into 0.25 x 1.0in strips in 1g portions with manual stirring. The aluminum will SLOWLY react with the nickel salt forming the metal Ni(s) through metathesis as a dark grey chunky powder which settles to the bottom. A gentle effervescence of hydrogen occurs during reaction. Add aluminum at a rate that maintains a steady effervescence and keeps temperature roughly in the 50°C range. Note this may take up to two hours! At the end of Al addition all green color from nickel salt should be discharged. If any color remains add another gram of aluminum and wait for soln to clear. Precipitated Nickel powder was added to 100ml 20% NaOH soln and manually stirred at 60°C for 30 min. Excess NaOH is decanted and nickel is washed with 5 x100ml aliquots of distilled water to remove excess base. At this point Urishubara nickel catalyst is prepared and ready for reduction.
Dissolve 5g pure phenylnitropropene in 50ml Ethanol and add to Ni solution.2 Now slowly add 3ml conc. HCl3 and 1 gram shredded aluminum w/ manual stirring. Aluminum will slowly dissolve with a more vigorous effervescence of hydrogen than the first step. Maintaining good stirring with a glass stirring rod is essential in beginning. Attempted magnetic stirring will result in frustration because nickel is ferromagnetic and will stick to stirbar preventing surface area exposure necessary for reduction. After aluminum is dissolved add three more milliliters HCl and one more gram Al. Repeat adding acid and Al until 10 grams Al and about 30ml HCl has been added. Aluminum reacts slowly. Expect addition to take about six hours, longer if temp falls below 50°C. Constant stirring towards end is not necessary, just give mix a good stir occasionally.
After all aluminum is added and mostly decomposed slowly pour in a soln of 30g NaOH in 100ml H2O with careful stirring. Wear goggles and be careful! Base neutralization is highly exothermic! In 30 minutes all aluminum sludge will solvate into bottom aqueous layer and a nice orange alcohol layer reeking of amine will settle out on top. Nickel is not dissolved by the NaOH so it will remain floating around between the two layers but this does not present a major problem. After all, it’s not poisonous like mercury or anything! Now decant off the top orange organic layer and distill off alcohol down to a orange stinky syrup completely different smelling than the P2NP. Dissolve these goodies in acetone and slowly add sulfuric acid to precipitate the amine sulfate. Voila!!!!!! about 3 grams light yellow amphetamine sulfate.
This is a very small scale and i would like to try this, but i am still interested in meanings from other people, who have experience in this kind of stuff.
I am a rookie and just at the beginning to understand everything what i had read the last two months. I am ready, got all equipment, which is needed, but before i start i would like to get the best knowlegde.
So, you're welcome to my first thread.
I looked at some Threads now and found nothing about amphetamine synthesis using urushibara (Nickel chloride & zinc dust(for example)
I had read how to convert Bmk glycidate to bmk oil, good information i did not know before.
But i would like to try a way without mercury chloride/nitrate.
NaBH4/CuCl2 is one option but better in large scale. It is the same for NiCl₂?
I know, the yield should not be as good as Al/Hg, but bmk is not very expensive, i can get it for aprox 70$ per kilo, so even if yield is only 30%, it would not be so bad as it sounds.
I found this informations about that Route:
(Maybe there a some ideas how to do it better)
Dissolve 4.0g Nickel Chloride hydrate (light green crystals) in 75 ml 95% ethanol w/ mag stirring and warming to 50°C. After salt is dissolved remove stir bar and add 1ml water and 1ml conc. HCl.1 While solution at 50°C slowly add 5g regular Reynolds wrap torn up into 0.25 x 1.0in strips in 1g portions with manual stirring. The aluminum will SLOWLY react with the nickel salt forming the metal Ni(s) through metathesis as a dark grey chunky powder which settles to the bottom. A gentle effervescence of hydrogen occurs during reaction. Add aluminum at a rate that maintains a steady effervescence and keeps temperature roughly in the 50°C range. Note this may take up to two hours! At the end of Al addition all green color from nickel salt should be discharged. If any color remains add another gram of aluminum and wait for soln to clear. Precipitated Nickel powder was added to 100ml 20% NaOH soln and manually stirred at 60°C for 30 min. Excess NaOH is decanted and nickel is washed with 5 x100ml aliquots of distilled water to remove excess base. At this point Urishubara nickel catalyst is prepared and ready for reduction.
Dissolve 5g pure phenylnitropropene in 50ml Ethanol and add to Ni solution.2 Now slowly add 3ml conc. HCl3 and 1 gram shredded aluminum w/ manual stirring. Aluminum will slowly dissolve with a more vigorous effervescence of hydrogen than the first step. Maintaining good stirring with a glass stirring rod is essential in beginning. Attempted magnetic stirring will result in frustration because nickel is ferromagnetic and will stick to stirbar preventing surface area exposure necessary for reduction. After aluminum is dissolved add three more milliliters HCl and one more gram Al. Repeat adding acid and Al until 10 grams Al and about 30ml HCl has been added. Aluminum reacts slowly. Expect addition to take about six hours, longer if temp falls below 50°C. Constant stirring towards end is not necessary, just give mix a good stir occasionally.
After all aluminum is added and mostly decomposed slowly pour in a soln of 30g NaOH in 100ml H2O with careful stirring. Wear goggles and be careful! Base neutralization is highly exothermic! In 30 minutes all aluminum sludge will solvate into bottom aqueous layer and a nice orange alcohol layer reeking of amine will settle out on top. Nickel is not dissolved by the NaOH so it will remain floating around between the two layers but this does not present a major problem. After all, it’s not poisonous like mercury or anything! Now decant off the top orange organic layer and distill off alcohol down to a orange stinky syrup completely different smelling than the P2NP. Dissolve these goodies in acetone and slowly add sulfuric acid to precipitate the amine sulfate. Voila!!!!!! about 3 grams light yellow amphetamine sulfate.
This is a very small scale and i would like to try this, but i am still interested in meanings from other people, who have experience in this kind of stuff.
I am a rookie and just at the beginning to understand everything what i had read the last two months. I am ready, got all equipment, which is needed, but before i start i would like to get the best knowlegde.
So, you're welcome to my first thread.
Is there a chance you can post the original source of that route?
