Hi I am currently trying to synthesis 5cl-adbb. I was given the instructions below. However I seem to be having issues. When I filter the liquid , nothing is being filtered via the filter paper. The Pottasium Carbonate does dissolve with the addition of cold water. However extraction of final product is impossible as the golden brown liquid just passes through the filter without leaving any final product. Any help would be appreciated.
1) ADBB precursor (main material)
2) Three auxiliary material:
DMF ( Cas: 68-12-2 )
Anhydrous Pottasium Carbonate ( Cas: 584-08-7)
Bromobutane ( Cas: 109-65-9 )
3) Tools:
Stainless Steel or Glass Reaction Bottle with stirring and heating function
PH Detector and disposable filter paper
Buchner Funnel;vaccum filtration kit;vacuum pump
1) ADBB precursor (main material)
2) Three auxiliary material:
DMF ( Cas: 68-12-2 )
Anhydrous Pottasium Carbonate ( Cas: 584-08-7)
Bromobutane ( Cas: 109-65-9 )
3) Tools:
Stainless Steel or Glass Reaction Bottle with stirring and heating function
PH Detector and disposable filter paper
Buchner Funnel;vaccum filtration kit;vacuum pump
I filtered it twice. I waited 2 hours, I saw mud at the bottom of the glass flask and it didn't want to be a stone. I poured excess water. a bowl of mud remained. 10 hours passed and there was a big stone in the bowl. I once made 100g 5cladba precursor plus the reduced 3 ingredients (2 powder, 2 liquid). you have better equipment, I think you will succeed.....
