Crude Acetaminophen Synthesis
Lab E: Adapted from Experiment #10
TA: Sudipta Biswas
Tuesday, 1:05pm
10/25/11
Sarah Kempkes
Abigail Scherer
Abstract:
The purpose of this experiment was to create and obtain pure acetaminophen. p-aminophenol and acetic anhydride were used to create acetaminophen and acetic acid. The acetic acid mixed with acetaminophen created an impure sample, which was purified through the addition of a water/methanol solution. The percent recovery of acetaminophen from the impure sample to the pure sample was 76%. The melting point of the pure sample was 167C - 169C.
Introduction:
Formulation of acetaminophen involves treating an amine with an acid anhydride to give rise to an amide. In this experiment, p-aminophenol, the amine, is treated with acetic anhydride to form acetaminophen, the amide.
The crude acetaminophen was expected to be dark in color. This was due to the fact that the impurities were formed from oxidation of the starting phenol. The intensity of this was enough to impart color to the crude acetaminophen.
Crude acetaminophen can be purified using the solid-liquid separation technique of ccrystallization where there is a transfer of the solute from the liquid solution to a pure solid crystalline phase. The pure acetaminophen will result in a white color, indicating impurities had been eliminated. …show more content…
Also added was 0.45mL water and 0.165mL acetic anhydride and a magnetic spin vane. An air condenser was attached to the vial and it was heated on an aluminum block, with a temperature maintained at 120C. After the solution dissolved, it was heated an extra 20 minutes to allow the reaction to go to completion then cooled back to room temperature. An ice bath was used to encourage crystal growth. The crystals were removed and centrifuged, then placed on a pre-weighed watch glass to dry and weigh. Percent recovery was found. A small sample was set aside for melting
TA: Sudipta Biswas
Tuesday, 1:05pm
10/25/11
Sarah Kempkes
Abigail Scherer
Abstract:
The purpose of this experiment was to create and obtain pure acetaminophen. p-aminophenol and acetic anhydride were used to create acetaminophen and acetic acid. The acetic acid mixed with acetaminophen created an impure sample, which was purified through the addition of a water/methanol solution. The percent recovery of acetaminophen from the impure sample to the pure sample was 76%. The melting point of the pure sample was 167C - 169C.
Introduction:
Formulation of acetaminophen involves treating an amine with an acid anhydride to give rise to an amide. In this experiment, p-aminophenol, the amine, is treated with acetic anhydride to form acetaminophen, the amide.
The crude acetaminophen was expected to be dark in color. This was due to the fact that the impurities were formed from oxidation of the starting phenol. The intensity of this was enough to impart color to the crude acetaminophen.
Crude acetaminophen can be purified using the solid-liquid separation technique of ccrystallization where there is a transfer of the solute from the liquid solution to a pure solid crystalline phase. The pure acetaminophen will result in a white color, indicating impurities had been eliminated. …show more content…
Also added was 0.45mL water and 0.165mL acetic anhydride and a magnetic spin vane. An air condenser was attached to the vial and it was heated on an aluminum block, with a temperature maintained at 120C. After the solution dissolved, it was heated an extra 20 minutes to allow the reaction to go to completion then cooled back to room temperature. An ice bath was used to encourage crystal growth. The crystals were removed and centrifuged, then placed on a pre-weighed watch glass to dry and weigh. Percent recovery was found. A small sample was set aside for melting