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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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preparation of aspirin typical a level procedure
Pear shaped flask
  • Bunsen burner
  • Reflux condenser
  • Vacuum filtration
Preparation of Aspirin (typical A level procedure)
slide4
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
The chemistry used to make aspirin

ethanoic

anhydride

2-hydroxybenzoic acid

aspirin

slide6
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?

slide7
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.)

slide8
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).

slide9
Preparation of Aspirin (typical A level procedure)

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

(A colourless liquid with a pungent smell).

slide10
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.

slide11
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.

slide12
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.

slide13
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
Heat under reflux for 30 minutes

140

120

°C

100

80

60

40

20

60

90

120

150

180

30

Time in minutes

slide15
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 minutes1
Heat under reflux for 30 minutes

140

120

°C

100

80

60

40

20

60

90

120

150

180

30

Time in minutes

slide17
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.

slide18
Preparation of Aspirin (typical A level procedure)

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

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