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I. Data

The document describes the synthesis of aspirin through the acetylation of salicylic acid with acetyl chloride. Tables show the characterization of starting materials and observations throughout the synthesis, including the addition of reagents, heating, crystallization, and testing of crude vs. recrystallized aspirin. The percent yield of crude aspirin was 142.53% and percent recovery after recrystallization was 115.77%, indicating impurities in the crude product. Melting point determination showed the crude aspirin had lower purity than literature values.

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Evander L. Batacan
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176 views3 pages

I. Data

The document describes the synthesis of aspirin through the acetylation of salicylic acid with acetyl chloride. Tables show the characterization of starting materials and observations throughout the synthesis, including the addition of reagents, heating, crystallization, and testing of crude vs. recrystallized aspirin. The percent yield of crude aspirin was 142.53% and percent recovery after recrystallization was 115.77%, indicating impurities in the crude product. Melting point determination showed the crude aspirin had lower purity than literature values.

Uploaded by

Evander L. Batacan
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOC, PDF, TXT or read online on Scribd
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I.

DATA

Table 11.1. Description of Chemicals.


Chemicals Description

Salicylic acid White homogenous powder


Acetyl chloride Clear homogenous liquid

Dil. Potassium Permanganate Red to violet homogenous liquid


Iodine solution Brown-reddish or yellowish brown liquid

Table 11.2. Observations on the Synthesis of Acetylsalicylic Acid.


Chemical Condition Observations

after addition of White heterogeneous liquid


Salicylic acid acetyl chloride
before heating White heterogeneous liquid

Mixture of salicylic acid, during heating White heterogeneous liquid


acetic anhydride and
phosphoric acid after heating White heterogeneous liquid

upon addition of Crystals mixed with water


water (there’s distinction of the water and the
solid salicylic acid)
upon placing in ice White heterogeneous liquid
bath
filtrate Clear homogenous liquid
Suction filtration
residue White powdery solid

Air- dried crystals White powdery solid

Equation for the Synthesis of Aspirin


Table 11.3. Weight and Percentage Yield of Crude Acetylsalicylic Acid.
Parameters Measurement

Mass of filter paper + watch glass 20.2g


Mass of filter paper + watch glass + aspirin 23.92g

Mass of crude aspirin 3.72g

Percent yield 142.53%

Table 11.4. Observations on the Recrystallization of Aspirin.


Conditions Observations

Crude aspirin + ethanol Clear heterogeneous with white crystals undissolved

Clear homogenous liquid


While heating
Crystals started to form
Addition of cold water
filtrate Clear homogenous liquid
Suction filtration
residue White solid crystals

Air- dried crystals White solid crystals

Table 11.5. Weight and Percent Recovery of Recrystallized Aspirin.


Parameters Measurement

Mass of watch glass 20g


Mass of watch glass + aspirin 23.01g

Mass of recovered aspirin 3.01g

Percent recovery 115.77%

Table of 11.6. Melting point Determination of Crude and Recrystallized Aspirin.


Conditions Crude Aspirin Recrystallized Aspirin

Melting Point range 160˚C N/A

Literature value of MP of Aspirin 136 ˚C

Percent purity, % 24% N/A


Table 11.7. Characterization of Starting Materials and Products.
Sample Tests and Observations

H2O (+,-) FeCl3 (+,-) Hot, acidic (+,-)


KMnO4
Salicylic acid Clear Clear Black to brown
heterogeneous - homogenous + homogenous +
liquid liquid liquid
Acetylsalicylic acid Clear Light violet Light brown
heterogeneous - heterogeneous - heterogeneous +
liquid liquid liquid
Commercially made Clear Light violet Light brown
Aspirin heterogeneous - heterogeneous - heterogeneous +
liquid liquid liquid

Table 11.8. Differentiation of Synthesized Aspirin and commercially- available Aspirin.


Sample Reaction of Iodine solution

Synthesized aspirin Brown heterogeneous liquid with white solids undissolved

Commercially- available aspirin Brown heterogeneous liquid with white solids undissolved

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