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  • PHA6115 Lab Experiment 1

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    This experiment involves the synthesis of methyl salicylate and aspirin through esterification reactions using salicylic acid, methanol, acetic anhydride, and sulfuric acid. The procedure for methyl salicylate synthesis involves heating a mixture of salicylic acid and methanol with sulfuric acid at 80°C for 15 minutes. For aspirin synthesis, salicylic acid is heated with acetic anhydride and phosphoric acid at 80°C for 15 minutes. Products are analyzed using odor tests, thin layer chromatography, and infrared spectroscopy. Purification is done through filtration and characterization helps identify the structures of the synthesized compounds.

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    This experiment involves the synthesis of methyl salicylate and aspirin through esterification reactions using salicylic acid, methanol, acetic anhydride, and sulfuric acid. The procedure for methyl salicylate synthesis involves heating a mixture of salicylic acid and methanol with sulfuric acid at 80°C for 15 minutes. For aspirin synthesis, salicylic acid is heated with acetic anhydride and phosphoric acid at 80°C for 15 minutes. Products are analyzed using odor tests, thin layer chromatography, and infrared spectroscopy. Purification is done through filtration and characterization helps identify the structures of the synthesized compounds.

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    52 views3 pages

    PHA6115 Lab Experiment 1

    Uploaded by

    The Dededo Native
    This experiment involves the synthesis of methyl salicylate and aspirin through esterification reactions using salicylic acid, methanol, acetic anhydride, and sulfuric acid. The procedure for methyl salicylate synthesis involves heating a mixture of salicylic acid and methanol with sulfuric acid at 80°C for 15 minutes. For aspirin synthesis, salicylic acid is heated with acetic anhydride and phosphoric acid at 80°C for 15 minutes. Products are analyzed using odor tests, thin layer chromatography, and infrared spectroscopy. Purification is done through filtration and characterization helps identify the structures of the synthesized compounds.

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    © All Rights Reserved
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    of 3

    University of Santo Tomas

    Faculty of Pharmacy
    PHA 6115 – Pharmaceutical and Medicinal Organic Chemistry

    EXPERIMENT 1
    SYNTHESIS OF METHYL SALICYATE AND ASPIRIN

    Materials:
    Equipment: Flasks or beakers, water bath, TLC apparatus, IR apparatus
    Chemicals: Salicylic acid, concentrated sulfuric acid, concentrated phosphoric
    acid, acetic anhydride, methanol

    Procedure for aspirin synthesis:


    1. Place 1g of salicylic acid and 2.5 mL of acetic anhydride in a small flask or
    beaker.
    2. Add 3 drops of concentrated phosphoric acid.
    3. Place the beaker/flask in the hood in a water bath at 80°C for 15 minutes
    4. Remove the beaker from the water bath. Add around 10-20 mL of water until
    turbidity forms.
    5. Pour contents of the beaker into a filtration setup. Vacuum or gravity filtration may
    be used.

    Procedure for methylsalicylate synthesis:


    1. Place 0.5g of salicylic acid and 3 mL of methanol in a small flask or beaker.
    2. Add 2 drops of concentrated sulfuric acid.
    3. Place the beaker/flask in the hood in a water bath at 80°C for 15 minutes, never
    going beyond such temperature (BP = ~65 °C).
    4. Note the odor before and after heating.

    Qualitative tests:
    1. Note the odor of the product. Compare this with the starting material.
    2. Run the solution on the FTIR. Obtain the IR spectra and save it for presentation
    to your lab instructor.
    University of Santo Tomas
    Faculty of Pharmacy
    PHA 6115 – Pharmaceutical and Medicinal Organic Chemistry

    EXPERIMENT 1: SYNTHESIS OF METHYLSALICYLATE AND ASPIRIN


    PRELAB QUESTIONS

    Names:
    Section and Group:

    1. Draw the equation for the reactions in the experiment. Label the structures and indicate their
    molecular weights. If there is more than one product, indicate which of those is the major
    product.
    -

    2. What is the mechanism of the reaction? What class of organic compounds react in this manner?
    - The mechanism of the reaction is esterification. The organic compounds carboxylic acid
    and alcohol react in this manner.

    3. The procedure states that the concentrated sulfuric acid must be added slowly. What happens if
    the acid is rapidly added in the experiment?
    - When sulfuric acid dissociates, heat is released. When done rapidly, the solution might
    splash out due to the rapid introduction of heat. (?)

    4. Why is purification necessary when doing organic synthesis? What are examples of purification
    methods? Will purification be done in this experiment?
    - Purification is necessary in order to remove impurities that may affect the reactivity of
    the involved compounds. Examples of purification methods are sublimation,
    crystallization, distillation, chromatography, and electrophoresis.

    5. Is purification also done in natural product experiments? What for?


    Natural product experiments also undergo purification. This is done for structure identification
    and quantity control of these natural products.

    6. What is the difference of the terms “purification” and “characterization”?

    7. Is infrared analysis a purification or characterization technique? Expound.


    University of Santo Tomas
    Faculty of Pharmacy
    PHA 6115 – Pharmaceutical and Medicinal Organic Chemistry
    8. What would be the problem if a sample with many impurities is immediately subjected to
    infrared analysis?

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