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need help converting 5449-12-7 and 20320-59-6
- Thread starter strangerdanger
- Start date
Middle layer? There are only 2 layers and the oil is the top one.
Yes around 11 liters:
- Steam distillation.
- Separate oil from water layer.
- Extract water phase with DCM.
- Dry with sodium sulfate and filter it.
- Evaporate DCM.
Yes around 11 liters:
- Steam distillation.
- Separate oil from water layer.
- Extract water phase with DCM.
- Dry with sodium sulfate and filter it.
- Evaporate DCM.
- By rothschild33
Will vacuum distillation work for the top layer instead of steam distillation?
↑View previous replies…
You do reaction with the phosphoric still in the BMK ? Or you wash with water?
What solvent on 1L, becuase baking soda is not very soluble in water unlike natrium chloride?
I have to measure the ph of my milk
Maybe i added to much water, but the problem is the 250ml water at the start wasn't enough to dissolve 500g of bmk powder
So i then added again 250ml of water, and then everything dissolved smoothly, after that when bmk dissolved in water
i added 720ml of phosphoric acid 75% to the flask, and proceed to boil reflux for 4 hours
after 1 hour there was already the oil on top, but i still made the reflux for 4 hours
and after it was finished, transparent-yellow oil was on top
But after washing it with water it became this milk color
i don't know why, and the yield is only 40% which is very bad i know this
Next time I will make experiment with: 300ml water, 500g powder and 1L of phosphoric acid 75%
what is your yield @Saul from 5449? 60-70% after washing with boiling water?
I tested 5449
5449/HCl 36%/H2O 1/1/1 4 hours in 90-95 C, I been advised by an expert to use less acid
5449/HCl 36%/H2O 1/1/1 4 hours in 90-95 C, I been advised by an expert to use less acid
One moll of your 5449 to one moll acid,and about 1,5 liter water per kilo 5449. Heath it up to about 50 to 70C ,and let it bubbel out the Co2. Bubbels stop (foaming) reaction done,
Sepp the two layers,top one is your oil,Wash it several times with boiling water and/or brine and dry over NaCi or dryed out epsom salt (in oven dryed) and your good for next step
Sepp the two layers,top one is your oil,Wash it several times with boiling water and/or brine and dry over NaCi or dryed out epsom salt (in oven dryed) and your good for next step
- By Berlin777
According to the experts a little bit excess of acid is needed in molar ratio. Also these temperatures didn't work for me and P2P crystallized few days later. I had to heat up to over 90 C. I will try your method as well as I haven't cooked too much P2P yet so it's worth to see what works best for me.
Post in thread 'p2p from bmk synthesis confirmed?' http://bbzzzsvqcrqtki6umym6itiixfhn...-from-bmk-synthesis-confirmed.6982/post-44159