PROCEDURE

WEAR GLOVES

1. Prepare a mixture of 5 mL conc HNO₃ and 5 mL conc H₂SO₄ in a 25 x 150mm test tube. Cool it to room temperature by means of a water bath, at your hood workstation.

2. To the tube, add 0.025 mole of your assigned halobenzene  over a period of about 5-10 min; gently swirling the tube to mix the contents after each addition.  Keep the reaction mixture between 50 - 55 ^oC.  DO NOT ALLOW THE REACTION MIXTURE TO EXCEED 60 ^oC.  The temperature may be controlled by allowing more time between the addition of successive  portions of halobenzene and by cooling the reaction flask as necessary with an ice water bath.

3. After the addition is completed and the exothermic reaction has subsided, heat the tube for 30 min. in a hot water bath,  maintaining the temperature in the reaction vessel below 60^oC during this period.  The settings on your hot plate should be between dial markings 2 & 3.

4. Cool the tube in an ice bath to room temperature.

5. Pour the reaction mixture into 50 mL of distilled water which is in a 150 mL beaker.

6. Isolate the crude product by vacuum filtration.

7. Wash the solid well with water.

8. Recrystallize the solid by dissolving it in a minimum amount of boiling solvent and allowing the solution to cool slowly.

9. Collect the crystals in a small Buchner funnel, and allow them to vacuum dry for several minutes.

10. Do thin-layer chromatography on your solid. Dissolve a very, very small amount of the product in acetone.

Dry a very tiny amount of your solid between two filter papers and determine the melting point range of your product,  compare it with the theoretical value.

Record the weight of your product.

Place what remians of your product in the waste jar(s) provided.

See "The Report" link on the web site for direction.