- Hits: 1328
PAA-Trials
There was 2 different trials for our PAA production:
-Trial 1 :
- Reflux 48g(16 mmol) methyl phenylacetate(45.3ml) and 200ml 2M NaOH for 2h.
- After the solution cools, acidify it with conc. HCl to reach a PH between 4.0 and 6.0, preferably 5.0.
- Extract three times with portions of ether equal to half the amount of solution present. The mixture must be stirred until any inorganic precipitate is dissolved.
- Filter the solution and separate the organic layer.
- Wash with cold water.
- Dry over anhydrous sodium sulfate.
- Distill the ether off. Diethyl ether boils at 34.6°C. Alternatively, leave the ether to evaporate.
- Recrystallize the residue from water to obtain free crystalline phenylacetic acid.
-Trial 2:
In this trial w proceed with acidification using concentrated hydrochloric acid, then filtration and recrystallization with cold water
- Reflux 48g(16 mmol) methyl phenylacetate(~45.3ml) and 200ml 2M NaOH for 2h.
- After the solution cools, acidify it with conc. HCl (~60mL). The pH value of the solution must be controlled between 4.0 and 6.0, preferably 5.0.
- Filtrate with a Vacuum filtration using cold water for washing.Purification:
- Recrystallize the solution by dissolving the filtrate in hot water then letting it cool down at room temperature before freezing overnight.
- Filter an dry the PAA produced
RESULTS:
PAA PRODUCTION RESULTS |
|||
YIELD |
MELTING POINT TEST |
||
WITHOUT PURIFICATION |
WITH PURIFICATION |
||
TRIAL1 |
37% |
75.4-76.3 |
66.6-70.4 |
TRIAL2 |
86% |
75-76.6 |
68.3-72.7 |
According to the melting point tests, trial 2was the best way used for PAA production with a high yield (86%) and the desired melting point (75-76.6) without purification also, so we can proceed for a large scale production.
There are several methods to identify the presence of phenylacetic acid other then melting point:
Solubility Test: Phenylacetic acid is soluble in hot water, ethanol and diethyl ether
Odor test: Phenylacetic acid has a characteristic odor of honey or horse sweat. If you suspect the presence of phenylacetic acid, you can smell the sample for this distinctive odor.