G.Patton
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what do you mean ?
6. 25% water solution of NaOH (8 liters) was added to reaction mixture and the phases were separated.
what do you mean ?
6. 25% water solution of NaOH (8 liters) was added to reaction mixture and the phases were separated.
but this aqueous layer is formed during the reaction. to separate and for scrap?
No, 2 layers is what you want.As the aq. layer gets saturated with water soluble salts it pushes the dillute isopropanol-freebase sol. out of the aq. layer.This property of isopropanol, as opposed to the other primary OH-s, to separate from water when salts are dissolved is exactly why it’s used in so many clandestine and otherwise syntheses.
Atleast I think so, hope I’m not talkin outta my ass
He means that you have to use separatory funnel
Atleast I think so, hope I’m not talkin outta my ass
If so I will now always salting my reaction mass before extraction with NaCl then I will have more less water to remove
Yes, it works great on my own experience
@btcboss2022 Did you maybe already made new batch bigger batch and documented it?
I am Interested in seeing your results and final yield of A oil that comes out of this reaction on let's say 1kg p2np scale
Hello,
I didn't do it yet again.
Thanks.
I tried your reaction, with 287g p2np and when the 30g of cucl2 was added all at once it was like volcano
after the eruption of fluid through the condenser and calming of my anger i putted the flask on hotplate
and let it heat for half hour, until all the cucl2 settled to bottom with some white layer
@btcboss2022 or @William Dampier how do you control the reaction to not go volcano style when adding cucl2 at once?
I tried this synthesis in 12L flask with liebig condenser, but it still wasn't enough big to stop the reaction going out of flask
How to control it?
And how large of flask-stainless reactor would one need for 1kg p2np reduction?
Respect the procedure next time, especially if it’s the first time you’re doing itor you’re unexperienced.It says dropwise.Do you have external cooling? Ice bath works great.
Thanks for answer, but i heard the most yields from this reaction were obtained when adding it at once, next time i will try to add it drop wise just to see difference
or maybe in two portions, so there will not be such big exotermic reaction
With this reaction i cooled it in water bath at times when it seemed to be to hot
@Mclssmxxl do you have experience with this reaction? in how many grams did you try this reaction and what was your yield of oil % at the end?
I tried your reaction, with 287g p2np and when the 30g of cucl2 was added all at once it was like volcano
after the eruption of fluid through the condenser and calming of my anger i putted the flask on hotplate
and let it heat for half hour, until all the cucl2 settled to bottom with some white layer
@btcboss2022 or @William Dampier how do you control the reaction to not go volcano style when adding cucl2 at once?
I tried this synthesis in 12L flask with liebig condenser, but it still wasn't enough big to stop the reaction going out of flask
How to control it?
And how large of flask-stainless reactor would one need for 1kg p2np reduction?
@btcboss2022 and @William Dampier
What color should the reaction be after the addition of cucl2 is completed and the reaction is finished?
Upper layer stays yellow and bottom(aqueous) layer is white, is this correct?
Or should both layers be transparent - white after the whole reaction is finished?
Because when I added NaOH into finished reaction the 2 layers formed, upper layer is yellow and bottom is white, is this good?
Or is yellow color of upper layer showing that there is still unreacted p2np inside of this layer?
If you got a vulcano adding the cucl2 if because you don't have enough solvent in the mixture possibly because in the previous steps you evaporate a lot of it, to avoid that you must do the previous steps in a flask or reactor to lose as low as possible the solvent.
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