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Lab and pilot plant tours Scaling up. www.abpischools.org.uk. Pear shaped flask Bunsen burner Reflux condenser Vacuum filtration. Preparation of Aspirin ( typical A level procedure). Preparation of Aspirin (typical A level procedure). 1. Weigh out 2g of

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Lab and pilot plant tours Scaling up

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Lab and pilot plant toursScaling up

www.abpischools.org.uk


  • Pear shaped flask

  • Bunsen burner

  • Reflux condenser

  • Vacuum filtration

Preparation of Aspirin (typical A level procedure)


Preparation of Aspirin (typical A level procedure)

1. Weigh out 2g of

2-hydroxybenzoic acid and place it in a pear shaped flask. (The starting material is a fluffy irritant white solid.)

2. Add 4.0cm3 of ethanoic anhydride.

(A colourless liquid with a pungent smell.)

3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.

4. When it is cool, add two anti-bumping granules.

5. Heat under reflux for 30 minutes.

6. Cool the mixture.

7. Pour into 100cm3 of cold water containing 10cm3 of dilute sulphuric acid. Stir and allow the resulting suspension to stand for 15 minutes.

8. Filter off the crystals that form. Dry and weigh the product.


The chemistry used to make aspirin

ethanoic

anhydride

2-hydroxybenzoic acid

aspirin


  • Preparation of Aspirin (typical A level procedure)

1. Weigh out 2g of

2-hydroxybenzoic acid and place it in a pear shaped flask. (The starting material is a fluffy irritant white solid.)

How would you do this for 20kg - 10,000 times the scale?


  • Preparation of Aspirin (typical A level procedure)

1. Weigh out 2g [20kg] of

2-hydroxybenzoic acid and place it in a pear shaped flask.

(The starting material is an irritant fluffy white solid.)


  • Preparation of Aspirin (typical A level procedure)

Temperature

probe

2. Add 4.0cm3 [40 litres] of ethanoic anhydride.

(A colourless liquid with a pungent smell).


  • Preparation of Aspirin (typical A level procedure)

2. Add 4.0cm3 [40 litres] of ethanoic anhydride.

(A colourless liquid with a pungent smell).


  • Preparation of Aspirin (typical A level procedure)

3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.


  • Preparation of Aspirin (typical A level procedure)

3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.


  • Preparation of Aspirin (typical A level procedure)

3. The reaction mixture will get slightly warm so cool it by swirling the flask under running water.


  • Preparation of Aspirin (typical A level procedure)

4. When it is cool, add two anti-bumping granules.

5. Heat under reflux for 30 minutes.


Heat under reflux for 30 minutes

140

120

°C

100

80

60

40

20

60

90

120

150

180

30

Time in minutes


  • Preparation of Aspirin (typical A level procedure)

5. Heat under reflux for 30 minutes.

Condenser

The maximum transfer of heat from the fluid in the jacket to the reaction mixture is 2° per minute


Heat under reflux for 30 minutes

140

120

°C

100

80

60

40

20

60

90

120

150

180

30

Time in minutes


Preparation of Aspirin (typical A level procedure)

Condenser

6. Cool the mixture.

7. Pour into 100cm3 [1000 litres] of cold water containing 10cm3 [100 litres] of dilute sulphuric acid. Stir and allow the resulting suspension to stand for 15 minutes.

8. Filter off the crystals that form. Dry and weigh the product.


  • Preparation of Aspirin (typical A level procedure)

8. Filter off the crystals that form. Dry and weigh the product.


Filter off the crystals that form


Dry and weigh the product


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