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Organic Chemistry III

Purification techniques and the aspirin preparation

  • 3 things to know
  • Papers 2 and 3

Overview

Reflux, washing, solvent extraction, recrystallisation and drying, simple and steam distillation, judging purity from melting and boiling temperatures, and preparing aspirin by acetylating 2-hydroxybenzoic acid with ethanoic anhydride, then purifying it and checking its purity.

What you need to know

Answer each one before you reveal it.

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Key term

During recrystallisation, why might hot filtration be performed before cooling?

Key term

How is crude aspirin purified after synthesis, and how is its purity assessed?

Key term

In recrystallisation, why is the impure solid dissolved in a minimum volume of hot solvent?

Questions from this subtopic

Each one with the model answer underneath.

  1. 1

    Define refluxing as a laboratory technique.

    Model answer

    Heating a reaction mixture continuously while vapours are condensed by a vertical condenser and returned to the flask, allowing prolonged heating without loss of volatile components.

  2. 2

    What is purification by washing in organic synthesis?

    Model answer

    Shaking the organic product with aqueous solutions in a separating funnel to remove water-soluble impurities.

  3. 3

    Define solvent extraction.

    Model answer

    A technique using a separating funnel to partition a compound between two immiscible solvents based on the compound's relative solubility in each solvent.

  4. 4

    In recrystallisation, why is the impure solid dissolved in a minimum volume of hot solvent?

    Model answer

    To ensure the solution is saturated, so that upon cooling, the maximum amount of pure product crystallises out.

  5. 5

    During recrystallisation, why might hot filtration be performed before cooling?

    Model answer

    To remove any insoluble impurities that would otherwise contaminate the crystals.

  6. 6

    What happens during the cooling stage of recrystallisation?

    Model answer

    The solution becomes supersaturated and pure crystals form slowly, while impurities remain dissolved in the solvent.

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