Question P2P phenylacetic acid synthesis without acetic anhydride?

kitboy

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Can anybody help me? Acetic anhydride is difficult to obtain and the easiest way to produce it is too contaminated with sulfur chlorides.
 

fidelis

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"Lead acetate definitely works, and am convinced that calcium acetate/phenylacetate is equally as effective. Iron salts are alleged to work for ketone synthesis from mixed carboxylic acids. But, the real answer is: Tube Furnace" (from this reddit post)

helpful vespiary discussion, if ur interested ^_^
 

Ranof

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Hello,

Probably in your country acetic anhydride is under strict control, without which you want to synthesize phenylacetone from phenylacetic acid.
Synthesis of acetic anhydride is simple, but if you don't have time for it, follow the method below.

Required materials
Phenylacetic acid
Acetic acid
Thorium oxide or manganese oxide
Nitrogen gas

First, build a furnace.
The way to build a furnace is as follows:
Connect a sep funnel to the adapter connecting to the condenser and place a mechanical stirrer inside the sep funnel.
Connect the nitrogen gas inlet tube to this part.
Fill the condenser with small stones cleaned with acetone (completely filled).
If you don't have stones, break a glass and fill it.
Pour manganese oxide or thorium oxide into these stones.
Connect an outlet adapter for nitrogen gas to the end of the condenser, which is connected to the discharge flask.

Middle part Heat the condenser with direct flame heat and slowly, while you are mixing phenylacetic acid and acetic acid (the stirrer in the sep funnel is stirring), open the sep valve and wait 15 minutes for every 3 shots that you direct the liquid into the condenser.

You will see phenylacetone coming out of the outlet, which of course is not pure, but you can distill it with vacuum or steam.

Tip (First pour the phenylacetic acid on the newspaper and place a fan in front of it because it quickly combines with the humidity in the air)

Adjust the amounts one by one.
For example, every 50 grams of phenylacetic acid requires at least 50 grams of acetic acid, but to be more sure, pour 57 grams of acetic acid.

The problem with this method is that thorium oxide is very expensive and difficult to find, but you may be able to find manganese oxide.
 
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