Phenylacetone (P2P) synthesis via BMK ethyl glycidate

[chem19]

@G.Patton
can you pls clarify that in step 14 "(14. After a while, distilled water 500 ml is added and the mixture is heated a little (no more than 60°C).".

My question is how long it should be heated. (Time duration) or any sign.
Thanks in advance.

 

[jotoy]

Hi and is it from this step that you stqrt if you have BMK 5449-12-7 powder or the new bmk powder in market now?

 

[chem19]

I started from Dimethylformamide, benzaldehyde exactly as in video.

 

[virus0815]

how much BMK glycidic acid (sodium salt) do i need for 1 gramm of P2P?

 

[61-50-7]

there is a little error : you said pmk instead of bmk in the first lines

 

[rampage]

Is the BMK glycidic acid (sodium salt) to water ratio 1:1 then add the hydrochloric acid to ph of 1?
if starting with BMK glycidic acid (sodium salt) is the ratio with water 1:1 then add the hydrochloric acid to ph of 1? then heat mixture and stir for 5hrs

 

[G.Patton]

Correct

 

[rampage]

found this article, is 80 degrees to warm? is 1kg of hydrochloric acid too much just add to reach ph1?

How to convert BMK powder to oil?(Below is just a general description of hydrolysis process, you may still need to contact us if you cannot get oil properly.)
1,1kg powder mix with 1kg warm water (around 80 degrees).
2, put in 1kg hydrochloric acid (HCL 37%) and you will see bubble generated.
3,Stirring the mixture for one hour and then stop.
4,After one more hour you will get oil layer in light yellow color.
5,Use separate funnel to retrieve oil.

 

[rampage]

hello
so as an example 1kg of bmk glycidic acid (sodium salt) and 1ltr of h2o are mixed, then hydrochloric acid is added to get a ph of 1.
then the rm is heated to 60 degrees and decarboxylated with constant stirring for 5hrs. then the heat and stirrer are turned off and the rm is transferred to a seperatory funnel where the layers are seperated.
top layer is p2p if the rm is still hot, or the bottom layer if rm is cold. so yield should be 1ltr of p2p?

 

[G.Patton]

No, ofc no. The yield is about 70-85%.
Moles, grams, litres and chemical calculations There is explanation how to calculate it.

 

[chem19]

@G.Patton
In step 7 what should be pH of the layer separated?
as I had 2 samples, one freshly collected which has pH of 6 and is light in colour 600ml. While remaining 400 ml which was collected after 2 months from standing solution has pH of 8. And is about 400ml and slight dark in colour.
Which solution should I proceed with. Fresh one or later one, or both. Plz suggest. Looking for guidance. Thanks in advance.

 

[G.Patton]

First of all, I would like to say Hello.
Its pH is not important at stage 7. You can use both of them.

 

[chem19]

Here are the picture

 

[chem19]

@G.Patton hello,
Need your blessings and support.
In step 6 NaOH solution 30% 450 ml is required.
I have NaOH pellet. How much of these pellet are needed with how much water, to make desirable 450 ml solution.
Plz guide me, as I m getting different different answers.
Thanks in advance
Regards

 

[chem19]

@G.Patton plz help me out, how to make 30% NaOH aq solution. Is it 30% w/w or w/c. Cauze chemicals are really costly, and a single wrong step may ruin whole process. Plz

 

[Throw-off]

Bro your over-thinking it. Look in Lab FAQ. Patton isn't gonna spoon feed you.

 

[chem19]

@Throw-off
Bro these are not hypothetical question, I m going through process, and these are refined problems that one who is going through wl face.
You just tell me in w/w and w/v, are you going to get same amount, huge difference,
Secondly after that to make pH 1 in another step while adding HCl is it not going to make difference. @G.Patton is here to guide us. So he will definitely going to spoon feed me and others. He is our mentor.
I m not arrogant, plz excuse me if you find so. But I m seriously looking for answer. I m in chemistry field from a long decade. So I know the importance of my questions. And this is not over thinking
Sorry if these text anyways made you think negative about me.

 

[Throw-off]

30g of sodium hydroxide and 70ml H2o.

There is a massive difference between guide and the coddle you expect from him. I think your the first chemist who has been in the game for a decade who can't work out how to make a sodium hydroxide 30% solution? So Bravo give yourself a pat on the back. If you've got yourself in such a state from hydrolysis perhaps the real question you should be asking is "is this for you?".

 

[G.Patton]

Water has 1g/1ml density, so that 1ml of distilled water can be counted as 1g.

 

[G.Patton]

Hello
450*0.3=135g of NaOH is loaded into the beaker, add there water to reach 450 ml risk.

 

[chem19]

@G.Patton Thank you so much. You are best. God bless you. If I succeed i will definitely contribute to your bb project. I wish if I could be your experimental chemistry student. Thank you so much again.

 

[Throw-off]

Anyone tried the new BMK Oil? cas 41232-97-7. A decade ago you could just get BMK powder make a solution with methanol 1:1 and drip it straight into the al/hg you would be done same day.. is hydrolysis required with all the new BMK derivatives? 5449 sodium salt sucks compared to the old school BMK.

 

[G.Patton]

You need to carry out alkaline hydrolysis and than acid one as for PMK glycidates.
It isn't true, you couldn't make meth from BMK glycidic acid sodium salt directly. You need to get P2P at first.

 

[Throw-off]

I'm not saying it was a sodium salt, I know it wasn't a sodium salt the texture of the powder looked totally different consistency from BMK derivative 5449.