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Tuco my friend,
I looked at the one pot synth recipe and the CuCl2/H2O solution is in 1/2 ratio meaning for 200mg CuCl2 you would use 400mg H2O as your solution proportion.
The temperature does not increase perhaps because it is such a small scale. Also you are using a two liter flask - kind of big for what you are working with, no?
After the CuCl2 solution is added, the temperature is maintained at 80c for 30 minutes with help of external heating. You got a hot plate you can dial in?
Add your NaOH solution to base. Seperate aqueous phase using IPA and reduce back into freebase with a vacuum.
Dissolve freebase into acetone and add H2SO4 until pH 6.
Place in freezer for ~12 hours
Collect salt and wash with cold dry acetone until it is white colored.
If you are still having trouble with these portions I would suggest using a larger batch. That is a 45 page thread, and it is not the only one. There has to be more info in there you can use. Read, brother.
I looked at the one pot synth recipe and the CuCl2/H2O solution is in 1/2 ratio meaning for 200mg CuCl2 you would use 400mg H2O as your solution proportion.
The temperature does not increase perhaps because it is such a small scale. Also you are using a two liter flask - kind of big for what you are working with, no?
After the CuCl2 solution is added, the temperature is maintained at 80c for 30 minutes with help of external heating. You got a hot plate you can dial in?
Add your NaOH solution to base. Seperate aqueous phase using IPA and reduce back into freebase with a vacuum.
Dissolve freebase into acetone and add H2SO4 until pH 6.
Place in freezer for ~12 hours
Collect salt and wash with cold dry acetone until it is white colored.
If you are still having trouble with these portions I would suggest using a larger batch. That is a 45 page thread, and it is not the only one. There has to be more info in there you can use. Read, brother.
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Let me tell you how to do it, first I will add 10ml ipa 80ml h2o, then I will add 3.5gr nabh4, then I will add 2gr p2np, not exceeding 60 degrees, then I will dissolve copper chloride 456mg in 1ml water and add it, not exceeding 80 degrees, then I will heat it to 80 degrees for 30 minutes, I will take the top layer and add the solution with 16ml water 25% naoh, then I will make ph 6 and put it in the freezer.