Hey guys,
We've finally succeeded in the lab with this synthesis.
First of all I have to say that we are no chemists, have no background in chemistry and have never synthesized any synthetic drug before. This is the first synthesis route we are trying.
We have had several tries so far that we kept to ourselves without sharing too much here. We quickly found out in what ways the lab needed to be improved to proceed with a successful synthesis.
We then took time to improve the cooling system, temperature control, ventilation and more aspects of the lab and got back to work just recently.
Just so that you know, the target product is purified freebase, not sulphate.
Synthesis report:
At this point unfotunately an issue occured as our vacuum pump can not be adjusted for the evaporation of water to be able to provide an accurate pressure.
We tried bringing water to boil at 0.04 MPa + 71.5 °C and played with the temperature in the levels between 71.5 - 90 °C but had to stop when it wouldn't boil.
The freebase:water (1:5) mixture is now sitting in a seperatory funnel until we have found a solution to this issue.
Current results (warning: pornographic content):
To be able to estimate the potency of the organic phases, that we have seperated and combined, we proceeded with carrying out two different crystalization processes.
First of all, we have so far produced 14L of organic phase from 800g of P2NP which we consider a big success after comparing this yield with fellow chemists from this forum. We are now storing this organic solution to carry out several experiments to learn more about the process.
Note: difference in colour comes from different mixing ratios of extracted aeqeous layer and firstly collected organic layer
1. 210ml freebase/ipa solution + 50ml anhydrous acetone + 99.99% sulphuric acid
Result: 7.2g of dried freebase (we messed up a little and spilled some product, yield should have been higher)
2. 200ml freebase/ipa solution + 99.99% sulphuric acid
Result: 7.3 of dried freebase
(this picture is not a picture of the dried sulphate)
The assumption here is that we are yielding Sulphate with around 60% - 61%.
Our goal is to find out how the addition of acetone is influencing the yield and also purity of the product.
So far we can say that the yield is not too much affected, we can not say too much about the purity yet as we haven't sent it to the lab yet. We will send it to the lab along a sample fo purified freebase once we got there. The sulphate that was crystalized without the use of acetone looks a little less white than the other but that's just an assumption..a quantitative lab test will tell more.
Freebase purification:
We were curious and wanted to find out how much purified freebase we could yield from the organic phase, per our estimations it should be approx 5% of the freebase/ipa solution which means that we should get approx 100ml actual freebase from 2L freebase/ipa solution.
We have carried out the evaporation of IPA in our rotovap. Here comes the tricky part, we did this step already in the past and it lead to us receiving a gooish, geelish honey like cream after the IPA was fully evaporated. Our assumption back then was that we have let it stay in the rotovap for too long, that's why we were more careful this time.
At the end of the evaporation process we could start seeing oily solid parts sticking to the distillation flask and assumed this might be our product + impurities:
We decanted the oily liquid into a beaker to view the results:
Strangely we have received 200ml instead of the estimated 100ml, we think this difference might come from impurities and us not drying the solution beforehand.
We then proceeded with adding water (on the picture you see 1:1 freebase:water ratio, we later stepped it up to 1:5) and shaking the solution in the flask to clean the flask and catch all solids/oil leftovers:
If you look closely, you can see oily parts floating in the water.
In the past we have had the same results and were able to produce a slightly milky freebase from this via a regular steam distillation.
We now wanted to put this to our rotovap when the above described issue occured.
We are right now stuck at this step and have stored the solution in a separatory funnel over night at room temperature (17 °C):
So far so good, we are curious to see what you guys think of our results and maybe what you would improve.
We are kinda happy with the so far produced results but need to find a way to make the distillation process of water work.
We are trying to get our hands on a very precise vacuum gauge for our vacuum pump to be able to provide a lower vacuum to manipulate the boiling point of water to lower levels around 28 - 40 °C. Another idea of ours is to further cool the water inside of the chiller as it reached 24.5 °C during the process as our chiller is not capable of holding it below 15 °C by himself.
As for the production of sulphate we are very happy as we are hitting (or even slightly exceeding) the yield from video tutorial and we are confident that we can achieve the same for the freebase production but we first need to get there, somehow.
Question:
1. When adding the IPA/Freebase solution to the rotovap we didn't had any issues with evaporating the IPA but when adding the freebase/water solution the pressure in the rotovap could not be held at the same level, although we have added the same volume of liquid for each process (1L each).
What could be the reason for this and how can we prevent this from happening?
2. What is your best and favourite way to go from impure freebase (after evaporating IPA) to a purified freebase (via steam distillation/ vacuum distillation/rotovap)
3. What ways do you prefer to remove IPA from the IPA/Freebase solution?
We think that it is not normal that we result in this honey like compound and assume that it should be more liquid.
4. It was recommended that we switch to a NaHCO3/Water wash instead of carrying out a distillation of the freebase:water solution to seperate the layers (followed by DCM extraction of water layer), what is your experience with this?
At this point I want to thank the professionals on this forum along other forum members that helped us to get to this point.
@G.Patton thanks for your amazing advice and help so far at all times of the day
@HEISENBERG thanks for providing this platform for beginners like myself to learn and meet like-minded people
@GhostChemist Thanks for providing more insight on the process and also for sharing your experience with us
@ImOutAlso Thanks for sharing your experience with us
@madmoney69 Thanks for the emotional support
@UWe9o12jkied91d Thanks for helping me with the steam distillation some weeks ago
That's it from me today, I wish you all an amazing start into the weekend.
Cincerly,
Koko