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  • Practical 22 - The Preparation of Aspirin

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    Joseph Kfoury
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    The document describes the preparation of aspirin through the esterification reaction of salicylic acid and ethanoic anhydride. The multi-step process involves: 1) refluxing the reactants to produce the crude aspirin product, 2) separating the product from the reaction mixture through filtration, 3) purifying the crude product via recrystallization, and 4) determining the yield and melting point of the purified product to assess its purity. Safety precautions are necessary due to the irritant and corrosive nature of some of the reactants.

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    The document describes the preparation of aspirin through the esterification reaction of salicylic acid and ethanoic anhydride. The multi-step process involves: 1) refluxing the reactants to produce the crude aspirin product, 2) separating the product from the reaction mixture through filtration, 3) purifying the crude product via recrystallization, and 4) determining the yield and melting point of the purified product to assess its purity. Safety precautions are necessary due to the irritant and corrosive nature of some of the reactants.

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    15 views3 pages

    Practical 22 - The Preparation of Aspirin

    Uploaded by

    Joseph Kfoury
    The document describes the preparation of aspirin through the esterification reaction of salicylic acid and ethanoic anhydride. The multi-step process involves: 1) refluxing the reactants to produce the crude aspirin product, 2) separating the product from the reaction mixture through filtration, 3) purifying the crude product via recrystallization, and 4) determining the yield and melting point of the purified product to assess its purity. Safety precautions are necessary due to the irritant and corrosive nature of some of the reactants.

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    © All Rights Reserved
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    Practical 22

    The Preparation of Aspirin

    (Core Practical 10a)

    Stage 1: Preparation of Crude Product

    Salicylic acid is an irritant


    Phosphoric acid is corrosive
    Ethanoic anhydride is flammable

    1. Place a 250 cm3 beaker, half-filled with water, on top of a tripod and gauze.

    2. Clamp a 50 cm3 round-bottomed flask so that it is partially submerged in the


    beaker of water, and fit a reflux condenser to it vertically. Start to run water
    through the condenser.

    3. Add two anti-bumping granules to the flask. Then weigh out 5.0 g of salicylic
    acid, 5.0 g of ethanoic anhydride, and 5.0 g of phosphoric acid into separate
    weighing bottles and add them, separately, into the flask through a funnel placed
    on top of the condenser.

    4. Heat the water in the beaker and reflux the mixture for 30 minutes. While this is
    happening, pour 150 cm3 of distilled water into a 250 cm3 beaker and place it in
    an ice bath.

    Stage 2: Separation of the product from the reaction mixture

    5. Allow the reaction mixture to cool down for a few minutes, then dismantle the
    condenser and pour the reaction mixture into the cold water. Stir for a few
    minutes and allow the mixture to settle.

    6. Filter the mixture through Buchner apparatus. Wash any residue remaining in the
    beaker into the funnel with more distilled water.

    7. Remove the filter paper with the solid residue on it and scrape it into another
    beaker.

    Stage 3: Purification of the crude product

    8. Recrystallise the aspirin from the minimum quantity of boiling water.


    Stage 4: Confirmation of yield and purity

    9. Once the product is dry, transfer it into a weighing bottle and weigh it.

    10. Determine the melting point of the sample.

    Questions:

    The structure of salicyclic acid is:

    a) Using structural formulae, write an equation for the reaction between salicylic
    acid and ethanoic anhydride.

    b) Work out your percentage yield.

    c) The melting point of pure aspirin is 135 oC. How pure is your sample? Explain
    how you know.

    d) Explain the main safety precautions you took during this experiment and why you
    took them.
    Recrystallisation – Purifying a Solid Organic Product

    Method Reason
    The solid is dissolved in the minimum
    possible quantity of hot solvent
    The solid should be soluble in hot
    solvent but not in cold solvent
    Filter through pre-heated funnel
    Allow to cool in an ice bath
    Filter under reduced pressure
    Wash the solid with a little cold solvent
    Dry the solid

    Melting Point Determination – Testing the Purity of the Product

    Method Reason
    Pack 1 cm of the solid as densely as
    possible into the sealed end of the
    capillary tube
    Place the capillary tube in the melting
    point apparatus.
    Ensure that the apparatus heats up very
    slowly as the expected melting point of
    the substance approaches
    Record the temperature when the liquid
    starts to melt
    Record the temperature when the liquid
    finishes melting
    Compare the melting point range to the
    known melting point of the pure solid

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