CHEM 219
Lab Report & Lab Notes
Experiment #: 6 Synthesis
Portage Learning
Inside you will get:
- Clear, Concise Scientific Language.
- All Tables and Figures Labelled Clearly.
- Included Units for All Measurements.
- Proofread Report.
- Portage Learning.
, Chemistry Lab Report
Experiment #: 6
Title: Synthesis
Purpose:
The purpose of the experiment is to synthesize and isolate cyclohexanone via a “green”
oxidation reaction and to determine if the green oxidant was a good choice for the
synthesis of cyclohexanone from cyclohexanol.
Procedure:
1. Add 16 mL of cyclohexanol (organic substrate) to the reaction vessel.
2. Add 7mL of glacial acetic acid. Use it to wash the remaining cyclohexanol from
the cylinder.
3. Stir the reaction gently and add an addition funnel (allows us to add the oxidizing
agent in a controlled fashion)
4. Add 100mL of bleach to the addition funnel.
5. Start the oxidation process by adding 25mL (quarter) into the mixture. Start a
slow drip that will add the remaining portion of bleach over a period of 15 minutes
6. After 15 minutes add another 100mL of bleach to the addition funnel and allow it
to slowly drip for another 15 minutes.
7. Once reaction has completed, use potassium iodide starch paper to check for
excess sodium hypochlorite. If excess bleach is present it will oxidize the paper
and the paper will turn blue.
8. Use universal indicating paper to test the ph. If neutral, add small quantity of
sodium hydroxide to raise the pH by a small amount.
9. Use a fractional distillation to isolate the cyclohexanone from the reaction
mixture.
10. Transfer the distillate into an Erlenmeyer flask and add 10g of sodium chloride
(table salt) and mix. The process is called salting out. Mix well and make sure
most of the salt has dissolved
11. Transfer the mixture to the separatory funnel (physically separates the 2 layers).
As the funnel narrows the layers become more pronounced.
12. Pour the cyclohexanone layer into a new flask. Use a small amount of sodium
sulfate as a drying agent.
13. After a short drying period, transfer the cyclohexanone to a vial by decanting the
pure solution away from the drying agent.
14. Add a small amount of the solution onto IR spectrometer sampling interface.
15. Make a dilution of the solution with an NMR solvent by mixing the a sample with
the solvent and mixing with the vortex. Add the mixture to the instrument (depth
gauge).
This study source
Chem219Exp6docx/
Lab Report & Lab Notes
Experiment #: 6 Synthesis
Portage Learning
Inside you will get:
- Clear, Concise Scientific Language.
- All Tables and Figures Labelled Clearly.
- Included Units for All Measurements.
- Proofread Report.
- Portage Learning.
, Chemistry Lab Report
Experiment #: 6
Title: Synthesis
Purpose:
The purpose of the experiment is to synthesize and isolate cyclohexanone via a “green”
oxidation reaction and to determine if the green oxidant was a good choice for the
synthesis of cyclohexanone from cyclohexanol.
Procedure:
1. Add 16 mL of cyclohexanol (organic substrate) to the reaction vessel.
2. Add 7mL of glacial acetic acid. Use it to wash the remaining cyclohexanol from
the cylinder.
3. Stir the reaction gently and add an addition funnel (allows us to add the oxidizing
agent in a controlled fashion)
4. Add 100mL of bleach to the addition funnel.
5. Start the oxidation process by adding 25mL (quarter) into the mixture. Start a
slow drip that will add the remaining portion of bleach over a period of 15 minutes
6. After 15 minutes add another 100mL of bleach to the addition funnel and allow it
to slowly drip for another 15 minutes.
7. Once reaction has completed, use potassium iodide starch paper to check for
excess sodium hypochlorite. If excess bleach is present it will oxidize the paper
and the paper will turn blue.
8. Use universal indicating paper to test the ph. If neutral, add small quantity of
sodium hydroxide to raise the pH by a small amount.
9. Use a fractional distillation to isolate the cyclohexanone from the reaction
mixture.
10. Transfer the distillate into an Erlenmeyer flask and add 10g of sodium chloride
(table salt) and mix. The process is called salting out. Mix well and make sure
most of the salt has dissolved
11. Transfer the mixture to the separatory funnel (physically separates the 2 layers).
As the funnel narrows the layers become more pronounced.
12. Pour the cyclohexanone layer into a new flask. Use a small amount of sodium
sulfate as a drying agent.
13. After a short drying period, transfer the cyclohexanone to a vial by decanting the
pure solution away from the drying agent.
14. Add a small amount of the solution onto IR spectrometer sampling interface.
15. Make a dilution of the solution with an NMR solvent by mixing the a sample with
the solvent and mixing with the vortex. Add the mixture to the instrument (depth
gauge).
This study source
Chem219Exp6docx/
