PMK Oil Synthesys From PMK (CAS 28578-16-7 Wax Form) Large Scale
- Thread starter btcboss2022
- Start date
1kg pmk ratio
1) 9.5L H2O with 500g sodium bicarbonate.
2) 1.4L H2O with 240g sodium hydroxide.
3) 1kg wax pmk.
4) 650g HCL
5) 2L DCM
Sir this ratio for 1kg wax pmk. Am i right?
1) 9.5L H2O with 500g sodium bicarbonate.
2) 1.4L H2O with 240g sodium hydroxide.
3) 1kg wax pmk.
4) 650g HCL
5) 2L DCM
Sir this ratio for 1kg wax pmk. Am i right?
Hi, if I don’t have a reactor would this work?
- Put 475 g of distilled h2o in a beaker and dissolve 25g of sodium bicarbonate
- 70 g distilled h2o into a boiling flask
- While stirring add 12 g sodium hydroxide
- Bring mixture up to 60c
- In a pot melt 50g of pmk wax
- Add to the h20 and sodium hydroxide mix
- Bring up to 80c slowly and reflux for an hour
- Add 3.25g Hcl 37% slowly- reflux for one hour at 80c while stirring
- After one hour- stop stirring and bring mixture down to 25c
- Separate water layer from oil
- Add oil layer back to boiling flask
- Add h20 and sodium mix from step 1- stir for 2-3 min
- Add 100g of dcm
- Allow separation for 15 min
- Distill dcm from solvent at 104f
- Collect mdp-2-p
- By Loki12
Of course you can use a boiling flask instead of a reactor. Not everyone here owns one, that is just fine as long as you can keep the temperature of your reaction where you need it - for example it is important to have an efficient cooling method, so that an exothermic reaction doesn't heat up too much and "escape" on you, which basically means the shit will fly out of your flask, can you imagine hot mixed solvents on your skin? It is also important to have a steady source of heat and a way to measure the temperature of the reaction itself, do not confuse this with how much temperature you are applying to the flask, you need something which will tell you the temperature of the solution inside and another something that will let you adjust the heat source in order to keep the reaction in the range of temperatures desired - good example is refluxing, if you cannot keep up a temperature and have a steady reflux going, most likely won't get good yields.
- By Loki12
Personally if you are just starting I would look at a "reaction flask" at least. A flask with three, best four heads - do yourself a favor and dedicate the middle for a mechanical overhead stirrer, they're cheap as hell and will allow you to proceed with reactions you will have great trouble attempting with a stirrer plate, not only will they make those so much easier, but you get cooling from the rapid stirring, quicker mixing of reagents, quicker escape of gasses due to the movement (great for example NABH4, you add too much with slow stirring, it will foam up out of the flask, but you turn up the crank on that overhead stirrer and make it go nuts, the reaction will proceed faster and will push out the gas out of the flask).
For heating, a heating mantle. Cheap with no stirring, get a mechanical one like I said, the combo will cost you less than a fancy heating mantle with stirring possibility.
For cooling, try to get a large inner diameter, USED dewar container. You can load them up with some dry ice, put your flask in one if it is small enough (1-2L) and you have sub-zero cooling for hours and hours.
And the method in this thread is solid. Thanks @btcboss2022 for posting it - I have used it myself, seems like a long time ago now.
If you are just a beginner in all this, at the end, don't separate the layers. No point in doing this. Do not use DCM either, you will have a hard time and a long time if you do not have a good source and good technique mastered, it is tough to work with for some. At the end, let the solution cool down after reflux, saturate all the water with salt (around 25g for every 100ml), check pH and add sodium bicarb slowly to raise the pH to near 7 - something around 4-5 should be good enough - the solution will be highly acidic, so it will be an exothermic reaction and it will foam up a lot, be careful (make sure you start when it has cooled down). The salt will make sure you won't pull much water with ethyl acetate which is a great substitute for DCM (remember EA will be on top, water on bottom, it does not behave like DCM). You shouldn't need much of the solvent anyway, the saturated salt water and the ketone after being lightly washed in alkaline should separate by itself. If you look past page 1 the author realized he was missing out on a lot of ketone by removing that layer, it was never fixed in the original post, but I remember myself the first time I tried this method, collecting that layer for later and adding NaOH followed by extraction; that worked too.
For heating, a heating mantle. Cheap with no stirring, get a mechanical one like I said, the combo will cost you less than a fancy heating mantle with stirring possibility.
For cooling, try to get a large inner diameter, USED dewar container. You can load them up with some dry ice, put your flask in one if it is small enough (1-2L) and you have sub-zero cooling for hours and hours.
And the method in this thread is solid. Thanks @btcboss2022 for posting it - I have used it myself, seems like a long time ago now.
If you are just a beginner in all this, at the end, don't separate the layers. No point in doing this. Do not use DCM either, you will have a hard time and a long time if you do not have a good source and good technique mastered, it is tough to work with for some. At the end, let the solution cool down after reflux, saturate all the water with salt (around 25g for every 100ml), check pH and add sodium bicarb slowly to raise the pH to near 7 - something around 4-5 should be good enough - the solution will be highly acidic, so it will be an exothermic reaction and it will foam up a lot, be careful (make sure you start when it has cooled down). The salt will make sure you won't pull much water with ethyl acetate which is a great substitute for DCM (remember EA will be on top, water on bottom, it does not behave like DCM). You shouldn't need much of the solvent anyway, the saturated salt water and the ketone after being lightly washed in alkaline should separate by itself. If you look past page 1 the author realized he was missing out on a lot of ketone by removing that layer, it was never fixed in the original post, but I remember myself the first time I tried this method, collecting that layer for later and adding NaOH followed by extraction; that worked too.