I have discovered something by accident in last night dream that might save you guys a lot of money!
If you use DMF as solvent/reaction media for Wacker you can VERY simply recycle
VERY expensive PdCl2!
After you are done with reaction use ordinary coffee filter and filter rxn contents.
There will be only a little filter cake, it is PdCl2 with some organic impurities.
Now wash it from the filter to the test tube, along what was left on the bottom of the baker.
Use acetone as the solvent.
Fill the test tube almost full of acetone, shake and let it settle.
Decant dark impure acetone (use syringe), let only last cm or so.
Fill it again, shake it, repeat the procedure at least 5 time.
You will have very pure PdCl2 left on the bottom after few washes.
You can now dry it and reuse it again. Works 100% for me!
I obtained more than 120g of ketone from recycled dried PdCl2 from 2 previous runs.
I was sloppy and recovered cca. 50%, but I am sure you can recover almost everything that didn't dissolve.
And make sure to dry it on the watch glass or something since it reacts with some metals.
I used acetone since it is cheap, dissolves all Wacker organic crap and doesn’t seems to dissolve PdCl2 much, if any.
This procedure works only with DMF as solvent and pure reactants(works great with bound_doublebound method p-benzo),
I think it is almost impossible to reuse it after MeOH synthesis, since there is
a lot of crap in the filter cake, but who knows...
Feel free to experiment like I did...
Try use different solvents, chill rxn contest and than extract etc.
Whatever you do just share it with others!
I know it might be very hard for you guys in EU and USA to find DMF, but it is worth money and effort!
I obtained mine as solvent for "old plastic models restoration".
It was used in the past as fast paint penetrator for some kind of now absolute plastic,
try in restoration institutes, art stores ,hobby shops etc.
Just UTFSE and make your own story!
I think it is almost impossible to reuse it after MeOH synthesis, since there is
a lot of crap in the filter cake, but who knows...
Feel free to experiment like I did...
I know it might be very hard for you guys in EU and USA to find DMF, but it is worth money and effort!
I obtained mine as solvent for "old plastic models restoration".
It was used in the past as fast paint penetrator for some kind of now absolute plastic,
try in restoration institutes, art stores ,hobby shops etc.
Just UTFSE and make your own story.
If you use DMF as solvent/reaction media for Wacker you can VERY simply recycle
VERY expensive PdCl2!
After you are done with reaction use ordinary coffee filter and filter rxn contents.
There will be only a little filter cake, it is PdCl2 with some organic impurities.
Now wash it from the filter to the test tube, along what was left on the bottom of the baker.
Use acetone as the solvent.
Fill the test tube almost full of acetone, shake and let it settle.
Decant dark impure acetone (use syringe), let only last cm or so.
Fill it again, shake it, repeat the procedure at least 5 time.
You will have very pure PdCl2 left on the bottom after few washes.
You can now dry it and reuse it again. Works 100% for me!
I obtained more than 120g of ketone from recycled dried PdCl2 from 2 previous runs.
I was sloppy and recovered cca. 50%, but I am sure you can recover almost everything that didn't dissolve.
And make sure to dry it on the watch glass or something since it reacts with some metals.
I used acetone since it is cheap, dissolves all Wacker organic crap and doesn’t seems to dissolve PdCl2 much, if any.
This procedure works only with DMF as solvent and pure reactants(works great with bound_doublebound method p-benzo),
I think it is almost impossible to reuse it after MeOH synthesis, since there is
a lot of crap in the filter cake, but who knows...
Feel free to experiment like I did...
Try use different solvents, chill rxn contest and than extract etc.
Whatever you do just share it with others!
I know it might be very hard for you guys in EU and USA to find DMF, but it is worth money and effort!
I obtained mine as solvent for "old plastic models restoration".
It was used in the past as fast paint penetrator for some kind of now absolute plastic,
try in restoration institutes, art stores ,hobby shops etc.
Just UTFSE and make your own story!
I think it is almost impossible to reuse it after MeOH synthesis, since there is
a lot of crap in the filter cake, but who knows...
Feel free to experiment like I did...
I know it might be very hard for you guys in EU and USA to find DMF, but it is worth money and effort!
I obtained mine as solvent for "old plastic models restoration".
It was used in the past as fast paint penetrator for some kind of now absolute plastic,
try in restoration institutes, art stores ,hobby shops etc.
Just UTFSE and make your own story.