P2P Synthesis via APAAN From Benzyl Cyanide

[Ranof]

APAAN Method with Visual Guide

Step 1: Weigh 12.8 grams of metallic sodium and cut it into small pieces (If not finely chopped, it will not dissolve properly).

Step 2: Transfer the sodium pieces into a round-bottom flask and attach a condenser to it.

Step 3: Slowly add 150 mL of absolute ethanol into the flask (You will observe the formation of many bubbles, indicating the release of hydrogen gas).

Step 4:Gently heat the sodium-ethanol mixture and activate the magnetic stirrer to help dissolve the sodium.

Step 5: Mix 50 grams of benzyl cyanide with 57.5 grams of ethyl acetate, and gradually add this mixture to the sodium ethoxide solution while stirring vigorously.

Step 6:Increase the stirring intensity. If the mixture becomes too viscous, add about 5 to 10 mL of ethanol.

Step 7:Set the temperature to 65°C and continue stirring for 3 hours (The solution will turn either orange or light yellow).

Step 8:After 3 hours, allow the mixture to thicken without stirring for a few minutes (It is recommended to leave it undisturbed for a full day).

Step 9: Mix 50 mL of distilled water with 25 mL of glacial acetic acid and bring the mixture to 70°C.

Step 10: Add the acidic solution to the main mixture and stir vigorously.

Step 11:Add 500 mL of hydrochloric acid to the solution (start with 300 mL initially).

Step 12: Turn on the magnetic stirrer and reconnect the condenser. Set the temperature to 100°C to heat and stir the acid-APAAN mixture (This process takes about 4 hours, during which a black oily BMK layer will slowly form).

Step 13:Add 100 mL of HCl every hour to improve the yield.

Step 14: Separate the top black oily layer using a separatory funnel.

Step 15:Use steam distillation to purify the phenylacetone.

Many thanks to @William D. and @G.Patton

 

[Blammo]

Why not just buy powdered sodium methylate

 

[Ranof]

Hello, do you mean sodium methoxide?

 

[Ranof]

Sodium methoxide
Sodium ethoxide
These two substances absorb moisture over time and their effectiveness decreases
It is better to prepare them freshly

 

[Ranof]

Your access to cheaper raw materials is very important.
In my area, sodium and ethanol are cheaper and more available than sodium ethoxide.

 

[Blammo]

Could you just use a small excess of sodium methoxide/ethoxide to account for any moisture?

If I understand correctly, water would react with the alkoxides to produce sodium hydroxide and the appropriate alcohol. So an excess of the alkoxide should, in my non-chemist opinion, account for any traces of moisture, whether in the solvent or alkoxide powder

 

[Ranof]

It is also related to time.
Perhaps a manufactured substance, for example, sodium ethoxide, can remain intact for a week or a month. If you take a GC test of the sample after this period, you will see that a lot of sodium hydroxide is found inside the substance.
This is due to the reaction with oxygen in the air.
That is why it is recommended to make and use its solution freshly, it gives better efficiency.