Hi Patton, I have tried to download this video, but it seems to be the benzaldehyde distillation one, and not the synthesis from benzyl alcohol as the title suggests.
"I don't have access to a vacuum pump, and I tried to distill benzaldehyde without it. The problem occurred with the rapid evaporation of the liquid before reaching the condenser. Shortly after vaporizing, the liquid condensed on the walls of the flask.""So, by using a heating mantle around the flask and a three-way distillation setup, I solved the problem. These components helped me overcome the issue I was facing during the distillation process."
"When I tried several times to make phenyl nitropropene using this method, I didn't get any results. Could it be possible that the benzaldehyde I produced using this approach had some issues?"
let me please point out, that with sodium-metabisulfite,
one can precipitate out the benzaldehyde as bisulfite-adduct. with subsequent re transformation ( here is my Potassium-Carbonate method, i use this also for the purification of Ketones or specifically Phenylacetone...)
Materials / Reagents:
Benzaldehyde-bisulfite adduct
Potassium carbonate (K₂CO₃)
Distilled water
Organic solvent (e.g., diethyl ether or dichloromethane)
Separatory funnel
Beaker or flask
Stirring rod or magnetic stirrer
Drying agent (e.g., anhydrous sodium sulfate or magnesium sulfate)
Funnel and filter paper
Rotary evaporator or distillation setup (optional, for solvent removal)
Procedure:
Place the benzaldehyde-bisulfite adduct in a beaker or flask.
Add enough distilled water to cover the solid and create a slurry.
Slowly add potassium carbonate (K₂CO₃) with stirring. Add in small portions to control foaming and avoid splashing.
As the potassium carbonate reacts, the adduct will break down, and free benzaldehyde will be liberated. Stir thoroughly to ensure complete reaction.
Once the evolution of gas (CO₂) subsides and the mixture turns cloudy or separates into layers, extract the liberated benzaldehyde using the organic solvent. Add the solvent, shake gently, and transfer the mixture to a separatory funnel.
Allow the layers to separate. Collect the organic (upper or lower layer depending on the solvent used) layer containing benzaldehyde.
Repeat the extraction 2–3 times with fresh solvent to ensure complete recovery.
Combine the organic extracts and dry them over anhydrous sodium sulfate or magnesium sulfate.
Filter off the drying agent.
Remove the solvent using a rotary evaporator or simple distillation to obtain pure benzaldehyde.
let me please point out, that with sodium-metabisulfite,
one can precipitate out the benzaldehyde as bisulfite-adduct. with subsequent re transformation ( here is my Potassium-Carbonate method, i use this also for the purification of Ketones or specifically Phenylacetone...)
Materials / Reagents:
Benzaldehyde-bisulfite adduct
Potassium carbonate (K₂CO₃)
Distilled water
Organic solvent (e.g., diethyl ether or dichloromethane)
Separatory funnel
Beaker or flask
Stirring rod or magnetic stirrer
Drying agent (e.g., anhydrous sodium sulfate or magnesium sulfate)
Funnel and filter paper
Rotary evaporator or distillation setup (optional, for solvent removal)
Procedure:
Place the benzaldehyde-bisulfite adduct in a beaker or flask.
Add enough distilled water to cover the solid and create a slurry.
Slowly add potassium carbonate (K₂CO₃) with stirring. Add in small portions to control foaming and avoid splashing.
As the potassium carbonate reacts, the adduct will break down, and free benzaldehyde will be liberated. Stir thoroughly to ensure complete reaction.
Once the evolution of gas (CO₂) subsides and the mixture turns cloudy or separates into layers, extract the liberated benzaldehyde using the organic solvent. Add the solvent, shake gently, and transfer the mixture to a separatory funnel.
Allow the layers to separate. Collect the organic (upper or lower layer depending on the solvent used) layer containing benzaldehyde.
Repeat the extraction 2–3 times with fresh solvent to ensure complete recovery.
Combine the organic extracts and dry them over anhydrous sodium sulfate or magnesium sulfate.
Filter off the drying agent.
Remove the solvent using a rotary evaporator or simple distillation to obtain pure benzaldehyde.
oh yes , i assume you hint that one, because my protocol is better in this thread ?? ( well i hope i am right, otherwise i look stupid because i 'll post it there r.now....lets let the fortune decide...)
