One-pot amphetamine synthesis from P2NP with NaBH4/CuCl2 (1kg scale)

[CasualChemist]

I tried the synthesis for a second time, wirteup of my first attempt is here: comment

This time I followed advice from @UWe9o12jkied91d and kept temperatures higher throughout the process. For the context my reaction is scaled down to 5 grams of P2NP.

First I pre-heated IPA+water mixture to 40 °C before adding NaBH4 (single batch). I omitted the ice/water bath completely and instead prepared a 120 mm computer fan pointed at the reaction flask. I added a spoon of fine grinded P2NP, temperature started rising and I turned the fan on when it reached 55 °C. I added next batch when temperature dropped to around 48 °C. I continued this procedure with temperature oscillating more or less in this range.

I waited for a minute and started adding CuCl2 solution.

On a side note, this time I made solution a bit more concentrated because I took into account that the original recipe mentioned 105 grams of CuCl2 in H2O and CuCl2x2H2O has ~27% bigger molar mass due to presence of water molecules, hence I used equivalent of 133 grams of CuCl2x2H2O in 200 ml of water.

With each addition of CuCl2 solution mixture foamed a lot and released brown precipitate which then turned into black flakes, like in the previous run. Temperature didn't rise too much so I placed the reaction flask in an oil bath and applied heating. With simultaneous heating and addition of CuCl2 temperature reached 72-74 °C, I was careful not to exceed 80 °C and used air cooling from time to time. Then I let it reflux at 75-78 °C for 30 minutes.

Unlike the previous run, after the reflux no layer separation occurred in the RM and I noticed distinct presence of an oily substance mixed with the RM. I tried filtering off the black dust with a filter paper but the mixture was so oily/thick it would barely go through filter paper so I just decanted the clear part and discarded the rest. I looked closer at the black residue and noticed two interesting things: tiny copper particles and oil patches floating on the surface.

Then I continued with NaOH, layer separation, phosphoric acid and so on.

This time again, my supposedly IPA+A-oil mixture didn't have a slightest yellow tint to it, it was colorless and a bit murky. Why in most of user reports A-oil is distinctly yellow? Most illustrations I found online including the Wikipedia page shows amphetamine freebase as a colorless liquid looking pretty much like what I've got. Does that depend on quality of P2NP crystals? I have a fairly fresh batch from nitrochemis.com and I keep in a fridge, crystals have very light yellow color.

Final product looks exactly like my previous batch, I didn't test it yet because I still have to do a wash.

Also I can't find any reference on how the final product should feel like when snorted. A ~100% pure product shouldn't burn at all? Does it make a difference if it's a phosphate or a sulfate? I'd be grateful if someone could describe actual sensation with high purity product.

 

[UWe9o12jkied91d]

I tried the synthesis for a second time, wirteup of my first attempt is here: comment

This time I followed advice from @UWe9o12jkied91d and kept temperatures higher throughout the process. For the context my reaction is scaled down to 5 grams of P2NP.

First I pre-heated IPA+water mixture to 40 °C before adding NaBH4 (single batch). I omitted the ice/water bath completely and instead prepared a 120 mm computer fan pointed at the reaction flask. I added a spoon of fine grinded P2NP, temperature started rising and I turned the fan on when it reached 55 °C. I added next batch when temperature dropped to around 48 °C. I continued this procedure with temperature oscillating more or less in this range.

I waited for a minute and started adding CuCl2 solution.

On a side note, this time I made solution a bit more concentrated because I took into account that the original recipe mentioned 105 grams of CuCl2 in H2O and CuCl2x2H2O has ~27% bigger molar mass due to presence of water molecules, hence I used equivalent of 133 grams of CuCl2x2H2O in 200 ml of water.

With each addition of CuCl2 solution mixture foamed a lot and released brown precipitate which then turned into black flakes, like in the previous run. Temperature didn't rise too much so I placed the reaction flask in an oil bath and applied heating. With simultaneous heating and addition of CuCl2 temperature reached 72-74 °C, I was careful not to exceed 80 °C and used air cooling from time to time. Then I let it reflux at 75-78 °C for 30 minutes.

Unlike the previous run, after the reflux no layer separation occurred in the RM and I noticed distinct presence of an oily substance mixed with the RM. I tried filtering off the black dust with a filter paper but the mixture was so oily/thick it would barely go through filter paper so I just decanted the clear part and discarded the rest. I looked closer at the black residue and noticed two interesting things: tiny copper particles and oil patches floating on the surface.

Then I continued with NaOH, layer separation, phosphoric acid and so on.

This time again, my supposedly IPA+A-oil mixture didn't have a slightest yellow tint to it, it was colorless and a bit murky. Why in most of user reports A-oil is distinctly yellow? Most illustrations I found online including the Wikipedia page shows amphetamine freebase as a colorless liquid looking pretty much like what I've got. Does that depend on quality of P2NP crystals? I have a fairly fresh batch from nitrochemis.com and I keep in a fridge, crystals have very light yellow color.

Final product looks exactly like my previous batch, I didn't test it yet because I still have to do a wash.

Also I can't find any reference on how the final product should feel like when snorted. A ~100% pure product shouldn't burn at all? Does it make a difference if it's a phosphate or a sulfate? I'd be grateful if someone could describe actual sensation with high purity product.

CasualChemistPure sulphate at least should not burn, i don't know about phosphate.There is discomfort due to fine particles irritating and tickling the mucosa, but after the fact it should not chemically burn.

 

[41Dxflatline]

Recrystallised nitrochemis p2np is lovely, before then though it REEKS of benzaldehyde and is a luminous canary yellow, A-Oil is 'yellow' because p2np is yellow and sometimes it doesn't all react

 

[KokosDreams]

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:

1. Solution IPA/H2O 2:1 (IPA: 4.8L Water: 2.4L) was added to the reactor and stirred at room temp.

2. NaBH4 (696,86g) was added at once while stirring.

3. P2NP (400g) was added in small portions but not too slow, so that the temperature of the mixture did not exceed 60 *С. Cooling in a waterbath was applied so that the mixture did not exceed 50.5 °C, the addition of P2NP was carried out as provocative as it was possible for us (20g initial load, continuing with 15g every 2 minutes). After the addition of P2NP the reaction was given 1h to finish before proceeding with the next step, we found this necessary due to the fast addition of P2NP

4. CuCl2 (42g) in water (80 ml) was added dropwise the temperature of the mixture did not exceed 80 *С.

5. Thereafter, reaction was then held at approx. 70 °C for 30 minutes using external heating with heating a heating mantle. To hold the mixture at 80 °C lead to the RM expanding/foaming too heavily which made us loose one batch, which is why we chose to not put it on 80 °C. The layers formed perfectly.

6. The mixture is filtered with Buchner funnel, using vacuum, to clean it from the solid waste of the CuCl2

7. Cold (Fridge temperature) 25% water solution of NaOH (Water: 2.4L, NaOH: 800g) was added to reaction until the reaction mass reaches a ph of approx. 11 and the mixture is stirred 5 min and once stirring stopped leave phases to seperate. To save time we carried out the phase seperation in a separatory funnel. The ph of the organic layer was 13 - 13.2

8. The organic layer is seperated

9. The organic layer is filtered using a Buchner Funnel + Vacuum

10. The aqueous phase was combined with the sludge and was thereafter extracted with 3.2L of IPA and put to settle to let the layers form perfectly

11. The organic layer from the aueqeous phase is collected and filtered using a Buchner + Vacuum

12. The seperated organic layers are mixed with the IPA extraction. Both collected organic layers are combined. We have decided to not dry the mixture this time as it previously lead to emulsions within the seperated organic layer when it was stored. Out assumption is that the Sodium Sulphate was stored wrong and therefore lost its anhydrous effect.

13. IPA was evaporated on vacuum to an oil using a rotavap (39 C°)

14. Water is added (1:5) to the oil to make steam distillation under vacuum using a rotovap.

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

 

[UWe9o12jkied91d]

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.
View attachment 11981View attachment 11982
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)
View attachment 11978View attachment 11979

2. 200ml freebase/ipa solution + 99.99% sulphuric acid
Result: 7.3 of dried freebase
View attachment 11980
(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:

View attachment 11983View attachment 11988

We decanted the oily liquid into a beaker to view the results:

View attachment 11984View attachment 11985

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:

View attachment 11986

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):

View attachment 11987

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

KokosDreamsIt’s hard to tell, in some of the pictures it looks like unreacted p2np, have you tried regular gravity filtration to isolate that solid?

on the other hand in some of the pictures it does have an oily look, it might be p2np turned oil with solvent due to heat that partially crystalized

Or it might be your pure amine that is degrading to this omega-fine white dust as freebase amines dr still freebase amine that gels up in the presence of water,so might be good to dry before

What I can add is that you do not use a rotovap as a faux steam distiller, you need to set up an apparatus either 1 flask or 2.Ideally for you based on what I have read would be to integrate a steam distillation in the process, distilling straight from reaction flask after naoh sol addition, skipping filtering of the solids, cutting back on manipulations and time.I would suggest you finally buy a mantle, it will make the difference compared to a plate for steam distill, especially for 20L.And I hear you barking, you have 1 neck only, just 2 way adaptor, center stirrer side condenser of choice, or just buy a stirred mantle if youre buying rotovaps

 

[KokosDreams]

It’s hard to tell, in some of the pictures it looks like unreacted p2np, have you tried regular gravity filtration to isolate that solid?

on the other hand in some of the pictures it does have an oily look, it might be p2np turned oil with solvent due to heat that partially crystalized

Or it might be your pure amine that is degrading to this omega-fine white dust as freebase amines dr still freebase amine that gels up in the presence of water,so might be good to dry before

What I can add is that you do not use a rotovap as a faux steam distiller, you need to set up an apparatus either 1 flask or 2.Ideally for you based on what I have read would be to integrate a steam distillation in the process, distilling straight from reaction flask after naoh sol addition, skipping filtering of the solids, cutting back on manipulations and time.I would suggest you finally buy a mantle, it will make the difference compared to a plate for steam distill, especially for 20L.And I hear you barking, you have 1 neck only, just 2 way adaptor, center stirrer side condenser of choice, or just buy a stirred mantle if youre buying rotovaps

UWe9o12jkied91dHey man, thanks for the extended feedback.

KokosDreamsIt’s hard to tell, in some of the pictures it looks like unreacted p2np, have you tried regular gravity filtration to isolate that solid?

I did had it sitting in a beaker for a while and I could see two different layers forming, I assumed the upper (more liquid) layer was probably water as I didn't dried it before or maybe even isopropyl that I haven't fully removed in the evaporation process of IPA

Does this makes sense?

Picture:

on the other hand in some of the pictures it does have an oily look, it might be p2np turned oil with solvent due to heat that partially crystalized

I hope we are talking about the above described compound (picture) when you are talking about 'solids'
It's consistency is actually like yummy honey, don't know how else to describe it

Or it might be your pure amine that is degrading to this omega-fine white dust as freebase amines dr still freebase amine that gels up in the presence of water,so might be good to dry before

I will definitely apply drying once I step into mass production, for this I will get a new batch of anhydrous sodium sulphate
I just left it out to prevent any complications to accure, which probably doesn't even makes sense

What I can add is that you do not use a rotovap as a faux steam distiller, you need to set up an apparatus either 1 flask or 2.Ideally for you based on what I have read would be to integrate a steam distillation in the process,

Interesting, I have seen videos online of 'essential oil extraction' with a rotovap ad figured it would make sense for me too, I also got it to work now and will post another report below my original comment in a few minutes

distilling straight from reaction flask after naoh sol addition, skipping filtering of the solids, cutting back on manipulations and time.

That is very interesting, I do believe in your experience and am always amazed when you do recommend me things I have never heard before elsewhere.
If I do distill straight from my 20L rbf I would need to skip on a second extraction of the sludge+aeqeous layer, correct?

I would suggest you finally buy a mantle, it will make the difference compared to a plate for steam distill, especially for 20L.

I actually have a 20L heating mantle in my lab for my 20L 3-Neck RBF, I just never thought of using this for an actual steam distillation as I only use this flask for the main reaction (NaBH4, P2NP, CuCL2) - very interesting

And I hear you barking, you have 1 neck only, just 2 way adaptor, center stirrer side condenser of choice, or just buy a stirred mantle if youre buying rotovaps

I feared a stirred mantle might cause issues when carrying out this very route as the sludge tends to get hard quickly, even when still in touch with fluids.
But I think there was a misunderstanding here as I do have 3 necks in my 20L RBF, or are you talking about my distillation set-up? This has a 2L RBF with 1 neck

I will post my updated results now.

 

[KokosDreams]

Update on the above posted synthesis report:

We got the rotovap to work to distill of the water by removing 50% of the solution that was put into the distillation flask, I have learned that high volumes of liquid might cause gases to build inside of the rotovap system that prevent a consistant application of vacuum.

I am now removing water (and hopefully freebase ) from the distillation flask at 40 °C

After a while a milky distllate started to collect inside of the receiving flask.
What was interesting is, that I could see crystal clear bubbles floating on top of the distillate, aswell as in the tap of the receiving flask. I firstly assumed that the crystal clear liquid was IPA, that wasn't fully removed before, but after removing it and smelling it, I do now think that it is my product. Another fact that might proof this theory is that it wasn't solluble in water.

Here a few pictures to further explain the current situation:

You can clearly see a liquid floating on top and also one being pushed into the tap at the bottom that is not solluble in water.
I assume that the water became milky as there might be freebase inside, that could now be removed with a DCM extraction.

Another interesting discovery I made was the look of the freebase/water sollution close to the end of the evaporation process:

I again assume that the oily/gooish liquid floating in the yellow/orange solution is our product, amphetamine freebase
When I had the same solution in a beaker and left a little of it in the beaker after decanting the whole solution into the distillation flask, it looked like this:

I now wonder if I massively failed or if I am on a good way receive amphetamine freebase from this
I honestly do have a good feeling and would proceed with a DCM extraction, then DCM evaporation to hopefully receive my product.

What do you guys think?

@UWe9o12jkied91d @G.Patton What do you guys think?

 

[41Dxflatline]

Funny you should post this, mine just finished refluxing. Is it supposed to be in layers? The black copper is in its own a small layer at the bottom of the flask

 

[KokosDreams]

Funny you should post this, mine just finished refluxing. Is it supposed to be in layers? The black copper is in its own a small layer at the bottom of the flask

41Dxflatline

Is it supposed to be in layers?

After what step exactly?

The black copper is in its own a small layer at the bottom of the flask

After the addition of the CuCL2/DH2O solution it is normla for the RM to seperate into layers.
Lower layer: dark/brown/red sludge with solids from the copper reaction
Top layer: yellowish/greenish colour depending on how the reaction worked out containing your product

In this case you continue with the upper layer, the lower layer can be used for an extraction with the aeqeous phase (+IPA) collected after adding 25%NaOH to the RM

 

[Marvyn]

Just curious. Would this reaction work with Nitromethane added shortly before the CuCl2 addition? Would it ruin the process or would you end up with MethAmp?

 

[Marvyn]

Last couple of times I’ve gotten green color. Frustrating since I thought I used much less Cucl2 this time. Tried extracting with a Xylene and got a dark green in the organic layer and a light green in the other layer. When washing with Dh20, it formed a gooey white bottom layer. Have no clue what could have gone wrong? Out of 4 attempts, only 1 was successful.

The green came upon basing. So it’s this because of unreacted Cu?

 

[UWe9o12jkied91d]

Last couple of times I’ve gotten green color. Frustrating since I thought I used much less Cucl2 this time. Tried extracting with a Xylene and got a dark green in the organic layer and a light green in the other layer. When washing with Dh20, it formed a gooey white bottom layer. Have no clue what could have gone wrong? Out of 4 attempts, only 1 was successful.

The green came upon basing. So it’s this because of unreacted Cu?

MarvynYes, temps? Time? Give us a rundown if you want help

 

[Marvyn]

UWe9o12jkied91d

So decided to keep it small until it’s figured out what’s going wrong.

120ml of IPA and 60ml of dh20 were added to a Rbf along with 11.5gr of Nabh4. This was left stirring from 10 mins while the 10gr of P2np was being crushed into a powder.

Once crushed, P2NP was added at approx 1gr per every 2-4 min. the temperature was 45c at the start and rose to 52c upon each addition. Once the temperature fell to approx 48c another addition was added. All 10gr of p2np was added in approx 15mins. Then temperature was brought up slowly to 55c and magnetic stirred until all color had disappeared (approximately 30mins). Shortly after approx 1.5-2gr of CuCl2 was dissolved in a minimal amount of dh20. Before the addition of Cucl another 2gr of Nabh4 was added to the mixture.
Then Cucl2 was added in 3 portions fairly quickly and the temperature never went above 60c. (After the second addition, I suspected It was already enough. But didn't want to not add enough) Once all cucl2 was added the temperature was slowly brought up to 76-78c and refluxed for 45mins. Shortly before the 45 mins it was noticed that most of the black solids fell to the bottom and a clear solution was being stired on top.
Once complete the mixture was vacuum filtered and 35% lab grade HCL was added and a white smoke evolved from the Rxn mixture. It took several dropper full of hcl to Finally get the mixture to acidic (much more than anticipated). Each time the flask was purged of the white smoke before adding more hcl. It seems like the solution did turn a slight blue color when the hcl was added..

After the solution was acidic distillation was setup and everything under 80c was distilled off. After that a solution of Koh in 70ml of dh20 was added to the to the original solution.. Once made basic is when the color went to a dark green. This was transferred to a step funnel and 70ml of Xylene was added and the mixture was shaken. The top Xylene layer turn dark green and the bottom water layer was a light green.

The bottom layer was decanted and the organic layer was washed with dh20. When added a white gooey substance came out into the water layer. This was repeated and each time some slimy substance remained into the h20. It also seemed like a salty substance was on the entire sup funnel walls. Which made me wonder if the Koh reacted with the Hcl after distillation and made Kcl. I would suspect this would be the case of no product was produced and the hcl remain in solution while the Ipa was distilled off. Even though the PH rose to approx after the distillation of the IPA?. Another thing to note. After the Koh solution was added it was noticed approx 25ml dark red oil went to the bottom of th flask.

This is the second time the green color has come to haunt me. First couple of times this hasn't been an issue. Only componats not lab grade this time was the Ipa and Xylene. But never had a problem with them in the past.

Any insight would be greatly appreciated.

 

[UWe9o12jkied91d]

UWe9o12jkied91d

So decided to keep it small until it’s figured out what’s going wrong.

120ml of IPA and 60ml of dh20 were added to a Rbf along with 11.5gr of Nabh4. This was left stirring from 10 mins while the 10gr of P2np was being crushed into a powder.

Once crushed, P2NP was added at approx 1gr per every 2-4 min. the temperature was 45c at the start and rose to 52c upon each addition. Once the temperature fell to approx 48c another addition was added. All 10gr of p2np was added in approx 15mins. Then temperature was brought up slowly to 55c and magnetic stirred until all color had disappeared (approximately 30mins). Shortly after approx 1.5-2gr of CuCl2 was dissolved in a minimal amount of dh20. Before the addition of Cucl another 2gr of Nabh4 was added to the mixture.
Then Cucl2 was added in 3 portions fairly quickly and the temperature never went above 60c. (After the second addition, I suspected It was already enough. But didn't want to not add enough) Once all cucl2 was added the temperature was slowly brought up to 76-78c and refluxed for 45mins. Shortly before the 45 mins it was noticed that most of the black solids fell to the bottom and a clear solution was being stired on top.
Once complete the mixture was vacuum filtered and 35% lab grade HCL was added and a white smoke evolved from the Rxn mixture. It took several dropper full of hcl to Finally get the mixture to acidic (much more than anticipated). Each time the flask was purged of the white smoke before adding more hcl. It seems like the solution did turn a slight blue color when the hcl was added..

After the solution was acidic distillation was setup and everything under 80c was distilled off. After that a solution of Koh in 70ml of dh20 was added to the to the original solution.. Once made basic is when the color went to a dark green. This was transferred to a step funnel and 70ml of Xylene was added and the mixture was shaken. The top Xylene layer turn dark green and the bottom water layer was a light green.

The bottom layer was decanted and the organic layer was washed with dh20. When added a white gooey substance came out into the water layer. This was repeated and each time some slimy substance remained into the h20. It also seemed like a salty substance was on the entire sup funnel walls. Which made me wonder if the Koh reacted with the Hcl after distillation and made Kcl. I would suspect this would be the case of no product was produced and the hcl remain in solution while the Ipa was distilled off. Even though the PH rose to approx after the distillation of the IPA?. Another thing to note. After the Koh solution was added it was noticed approx 25ml dark red oil went to the bottom of th flask.

This is the second time the green color has come to haunt me. First couple of times this hasn't been an issue. Only componats not lab grade this time was the Ipa and Xylene. But never had a problem with them in the past.

Any insight would be greatly appreciated.

MarvynDon't stop to wait for anything after p2np addition, add copper right after, stop cooling so much, cool if you've got foaming runaway reaction or once youve reached 70c at any time before Cu addition, even then do so just a bit, at your scale things are cooling down quite fast.
Why are you acidifying with HCl? It is not needed, if you do everything right and let the reaction take place most of your bubbling should be over by the time flask has reached RT after reflux.You proceed to basify as normal and you know the rest, you don't have to overcomplicate things for free.

 

[Marvyn]

Don't stop to wait for anything after p2np addition, add copper right after, stop cooling so much, cool if you've got foaming runaway reaction or once youve reached 70c at any time before Cu addition, even then do so just a bit, at your scale things are cooling down quite fast.
Why are you acidifying with HCl? It is not needed, if you do everything right and let the reaction take place most of your bubbling should be over by the time flask has reached RT after reflux.You proceed to basify as normal and you know the rest, you don't have to overcomplicate things for free.

UWe9o12jkied91dI added the Hcl so I could distill off the IPA because I planned on extracting with a NP.
When I did base and got the IPA layer per first instructions. It looked like it worked perfect. Got product to come out of solution. But when the product that precipitated seemed to be all salts. That’s why I’ve been trying another method to extract. But I will give it another shot and hopefully get something. Thanks for you help.

 

[41Dxflatline]

UWe9o12jkied91d

So decided to keep it small until it’s figured out what’s going wrong.

120ml of IPA and 60ml of dh20 were added to a Rbf along with 11.5gr of Nabh4. This was left stirring from 10 mins while the 10gr of P2np was being crushed into a powder.

Once crushed, P2NP was added at approx 1gr per every 2-4 min. the temperature was 45c at the start and rose to 52c upon each addition. Once the temperature fell to approx 48c another addition was added. All 10gr of p2np was added in approx 15mins. Then temperature was brought up slowly to 55c and magnetic stirred until all color had disappeared (approximately 30mins). Shortly after approx 1.5-2gr of CuCl2 was dissolved in a minimal amount of dh20. Before the addition of Cucl another 2gr of Nabh4 was added to the mixture.
Then Cucl2 was added in 3 portions fairly quickly and the temperature never went above 60c. (After the second addition, I suspected It was already enough. But didn't want to not add enough) Once all cucl2 was added the temperature was slowly brought up to 76-78c and refluxed for 45mins. Shortly before the 45 mins it was noticed that most of the black solids fell to the bottom and a clear solution was being stired on top.
Once complete the mixture was vacuum filtered and 35% lab grade HCL was added and a white smoke evolved from the Rxn mixture. It took several dropper full of hcl to Finally get the mixture to acidic (much more than anticipated). Each time the flask was purged of the white smoke before adding more hcl. It seems like the solution did turn a slight blue color when the hcl was added..

After the solution was acidic distillation was setup and everything under 80c was distilled off. After that a solution of Koh in 70ml of dh20 was added to the to the original solution.. Once made basic is when the color went to a dark green. This was transferred to a step funnel and 70ml of Xylene was added and the mixture was shaken. The top Xylene layer turn dark green and the bottom water layer was a light green.

The bottom layer was decanted and the organic layer was washed with dh20. When added a white gooey substance came out into the water layer. This was repeated and each time some slimy substance remained into the h20. It also seemed like a salty substance was on the entire sup funnel walls. Which made me wonder if the Koh reacted with the Hcl after distillation and made Kcl. I would suspect this would be the case of no product was produced and the hcl remain in solution while the Ipa was distilled off. Even though the PH rose to approx after the distillation of the IPA?. Another thing to note. After the Koh solution was added it was noticed approx 25ml dark red oil went to the bottom of th flask.

This is the second time the green color has come to haunt me. First couple of times this hasn't been an issue. Only componats not lab grade this time was the Ipa and Xylene. But never had a problem with them in the past.

Any insight would be greatly appreciated.

MarvynWhat Marvyn said, also this is a minor thing but you should add the copper as a solid having it in solution makes the initial reaction more vigorous and can cause it to foam over

 

[Marvyn]

What Marvyn said, also this is a minor thing but you should add the copper as a solid having it in solution makes the initial reaction more vigorous and can cause it to foam over

41DxflatlineWould adding to much Cucl2 make the green color come through after extraction?

 

[41Dxflatline]

Would adding to much Cucl2 make the green color come through after extraction?

Marvynyes