SWIM started with[cas 5449-12-7] after 4h of heating got aqueous layer on top and oily bottom... what did wrong? too much acid?
further attempts with cas 5449-12-7 and step 1 of described method gave proper and stable results!
P2P synthesis from BMK glycidate ethers
- Thread starter G.Patton
- Start date
Hi, could you answer some doubts?
3.- What is the pH in this stage after wahsing with DCM? The wash with brine is mandatory? If yes, what is the concentration of NaCl solution?
4.- This is simple distilation at DCM boling point (around 40ºC) rigth?
P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
1.- What is the point of mixing with water (65 ml), and distill again to separete from water? or could we have some unwanted components?
What is the pressure and the temperature in this stage for the vacuum distilation?
Is possible simple distilation without vacuum? Around water boiling point (100ºC)
3.- What is the pH in this stage after wahsing with DCM? The wash with brine is mandatory? If yes, what is the concentration of NaCl solution?
4.- This is simple distilation at DCM boling point (around 40ºC) rigth?
P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
1.- What is the point of mixing with water (65 ml), and distill again to separete from water? or could we have some unwanted components?
What is the pressure and the temperature in this stage for the vacuum distilation?
Is possible simple distilation without vacuum? Around water boiling point (100ºC)
- By G.Patton
>3
25% NaCl aq is okay and yes. It is necessary.
>4
Yes, you are right. You can use rotovap.
>P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
yes, it is necessary. I can't say for sure. The difference can vary greatly.
>1.- What is the point of mixing with water (65 ml), and distill again to separete from water?
read about steam distillation in Lab FAQ section
>What is the pressure and the temperature in this stage for the vacuum distilation?
Is possible simple distilation without vacuum? Around water boiling point (100ºC)
Depends on vacuum, I can't answer you. I think it is impossible, you'll spoil your p2p with height temperature (probably).
25% NaCl aq is okay and yes. It is necessary.
>4
Yes, you are right. You can use rotovap.
>P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
yes, it is necessary. I can't say for sure. The difference can vary greatly.
>1.- What is the point of mixing with water (65 ml), and distill again to separete from water?
read about steam distillation in Lab FAQ section
>What is the pressure and the temperature in this stage for the vacuum distilation?
Is possible simple distilation without vacuum? Around water boiling point (100ºC)
Depends on vacuum, I can't answer you. I think it is impossible, you'll spoil your p2p with height temperature (probably).
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- By Costa
Hi!
I made this process, and after this step:
"2. Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered."
This is what I have obtained (see the picture below). Is this the expected aspect of the reaction? and my question is: is this top layer already P2P? should I put aside this layer (and keep it) and add DCM to the rest (bottom layer) in order to extract the remaining P2P from there?
Many thanks in advance!
I made this process, and after this step:
"2. Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered."
This is what I have obtained (see the picture below). Is this the expected aspect of the reaction? and my question is: is this top layer already P2P? should I put aside this layer (and keep it) and add DCM to the rest (bottom layer) in order to extract the remaining P2P from there?
Many thanks in advance!
Last edited by a moderator:
- By Costa
Hi, I followed the procedure step by step as mentioned in the instructions and it didn't work. I made several extractions of the "water" (bottom layer) using DCM and once I combined them (pouring over the P2P layer), there was some kind of reaction because lot of solids appeared. Anyway, I continued with the procedure, just in case; so I add the brine (NaCl + water) and it was even worst...
In your last message you told I should add DMC and brine at the same time, so today I will try following this method.
You told I have to check the pH of the brine; what is "brine" refers to? is it the layer with NaCl (the remaining layer once I separate the oily layer with P2P)? the addition of the NaCl is just to rise the pH? why is NaCl used instead if NaOH for this objective?
In your last message you told I should add DMC and brine at the same time, so today I will try following this method.
You told I have to check the pH of the brine; what is "brine" refers to? is it the layer with NaCl (the remaining layer once I separate the oily layer with P2P)? the addition of the NaCl is just to rise the pH? why is NaCl used instead if NaOH for this objective?
- By G.Patton
Hi.
I have no idea what is it, have you checked your precursor? What are you use for this synthesis?
I wrote that you have to add them in one separatory funnel, there is no difference of addition sequence.
You can use distilled water for washing of your extract. Brine (NaCl aq solution) is used in order to rinse acid trace from your P2P extract. It's easy, cheap and safe. Also, it is more convenient to separate layers with brine. You have to wash the organic extract by brine until neutral pH 7.
I have no idea what is it, have you checked your precursor? What are you use for this synthesis?
I wrote that you have to add them in one separatory funnel, there is no difference of addition sequence.
You can use distilled water for washing of your extract. Brine (NaCl aq solution) is used in order to rinse acid trace from your P2P extract. It's easy, cheap and safe. Also, it is more convenient to separate layers with brine. You have to wash the organic extract by brine until neutral pH 7.
I have no idea what is it, have you checked your precursor? What are you use for this synthesis?
i used: cas 5449-12-7. I took off the P2P layer and with the rest, I made the extractions with DCM. Each extraction (the oily layer obtained when adding DCM), I combined them with the P2P. It was then when the precipitate appeared.
Today I will not combine the P2P with the extractions, just in case... I will made the extractions with DCM and each extract, I will wash them with brine, as you told. Lets see what happens.
thanks
i used: cas 5449-12-7. I took off the P2P layer and with the rest, I made the extractions with DCM. Each extraction (the oily layer obtained when adding DCM), I combined them with the P2P. It was then when the precipitate appeared.
Today I will not combine the P2P with the extractions, just in case... I will made the extractions with DCM and each extract, I will wash them with brine, as you told. Lets see what happens.
thanks
Hi, as said, I repeated the process following the instructions of the document (and your comments) step by step. I got exactly the same product on this step:
I took the oily layer (top layer, which has P2P) and once it cooled down after 10 minutes it has this aspect:
.
Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:
as you can see, there was some kind of white precipitate on the bottom, there were not two layers, just the white solids and the rest.
What did I do wrong? The document is not very clear...
Many thanks in advance and sorry for that many questions, but this process it is being a headache...
Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:
What did I do wrong? The document is not very clear...
Many thanks in advance and sorry for that many questions, but this process it is being a headache...
- By G.Patton
It is quite strange. Check cas 5449-12-7 mp. Also, you can take the solid orange "p2p oil" from your beaker (take couple grams) and dissolve in water at room temperature or with slight heating (about 30 deg C). I think that this solid is water soluble salt. If you'll get oily layer on the top, I am right.