Liquid-liquid extraction is used here to purify the mixture obtained at the end of the reaction. For your respective reaction the different species potentially found in solution at the end of the reaction to partition between the organic and aqueous layers during the liquid-liquid extraction step? Explain your prediction. Oxone), how you would expect

EBK A SMALL SCALE APPROACH TO ORGANIC L
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Chapter80: Crystallization: Purification Of Solids
Section: Chapter Questions
Problem 4P
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REACTION
1. Using a burette, measure the cyclohexene (6.0 mmol) and transfer to
a 125 mL erlenmeyer, along with acetone ([Cyclohexene] = 1 M). Add
a stirbar.
2. Cool the solution in an ice-bath for 10 minutes with magnetic stirring.
3. Meanwhile, in a 2nd 125 mL erlenmeyer, dissolve Oxone (15.6 mmol) in
deionized water ([Oxone] = 0.60 M).
4. Attach a ring-clamp right over your flask. Add a closed separatory
funnel, such that the bottom tip is partially inserted in the flask.
5. Add your Oxone solution into the separatory funnel.
6. When your cyclohexene solution is sufficiently cold, gently open the
bottom valve of the separatory funnel to add the Oxone solution.
Adjust the valve to obtain a flow of approximately 1–2 drops/second.
7. Once the addition is complete, rinse the sepa
millilitres of water.
ory funnel with a few
8. Remove the flask from the ice bath, and allow the reaction to stir at
room temperature for 20 minutes.
9. After 20 minutes, add 12.5 M HCI (14.9 mmol) dropwise to the stirring
solution. Allow the reaction to stir for 10 minutes before proceeding
with liquid-liquid extraction (p.8).
PURIFICATION– LIQUID-LIQUID EXTRACTION
1. Assess the success of your reaction by performing a TLC on your crude reaction mixture. (See TLC
protocol below for details)
2. Pour your resulting reaction mixture into 30 mL of water in a separatory funnel.
3. Add 5 mL of ethyl acetate, and shake vigorously.
|4. Drain the aqueous and organic layers into separate erlenmeyer flasks.
5. Return the aqueous layer to the separatory funnel. Extract it two more times with additional 5 mL portions
of ethyl acetate, mixing well.
|6. Drain the final aqueous layer. Add all of the organic fractions back into the separatory funnel.
7. Wash the combined organic phase by adding 5 mL of clean water to the separatory funnel and mixing well.
8. Drain both layers separately into their respective erlenmeyers.
9. Analyze the purified organic extract by TLC using the protocol below.
9) Liquid-liquid extraction is used here to purify the mixture obtained at the end of the
reaction. For your respective reaction
the different species potentially found in solution at the end of the reaction to partition
between the organic and aqueous layers during the liquid-liquid extraction step? Explain
your prediction.
Oxone), how you would expect
Transcribed Image Text:REACTION 1. Using a burette, measure the cyclohexene (6.0 mmol) and transfer to a 125 mL erlenmeyer, along with acetone ([Cyclohexene] = 1 M). Add a stirbar. 2. Cool the solution in an ice-bath for 10 minutes with magnetic stirring. 3. Meanwhile, in a 2nd 125 mL erlenmeyer, dissolve Oxone (15.6 mmol) in deionized water ([Oxone] = 0.60 M). 4. Attach a ring-clamp right over your flask. Add a closed separatory funnel, such that the bottom tip is partially inserted in the flask. 5. Add your Oxone solution into the separatory funnel. 6. When your cyclohexene solution is sufficiently cold, gently open the bottom valve of the separatory funnel to add the Oxone solution. Adjust the valve to obtain a flow of approximately 1–2 drops/second. 7. Once the addition is complete, rinse the sepa millilitres of water. ory funnel with a few 8. Remove the flask from the ice bath, and allow the reaction to stir at room temperature for 20 minutes. 9. After 20 minutes, add 12.5 M HCI (14.9 mmol) dropwise to the stirring solution. Allow the reaction to stir for 10 minutes before proceeding with liquid-liquid extraction (p.8). PURIFICATION– LIQUID-LIQUID EXTRACTION 1. Assess the success of your reaction by performing a TLC on your crude reaction mixture. (See TLC protocol below for details) 2. Pour your resulting reaction mixture into 30 mL of water in a separatory funnel. 3. Add 5 mL of ethyl acetate, and shake vigorously. |4. Drain the aqueous and organic layers into separate erlenmeyer flasks. 5. Return the aqueous layer to the separatory funnel. Extract it two more times with additional 5 mL portions of ethyl acetate, mixing well. |6. Drain the final aqueous layer. Add all of the organic fractions back into the separatory funnel. 7. Wash the combined organic phase by adding 5 mL of clean water to the separatory funnel and mixing well. 8. Drain both layers separately into their respective erlenmeyers. 9. Analyze the purified organic extract by TLC using the protocol below. 9) Liquid-liquid extraction is used here to purify the mixture obtained at the end of the reaction. For your respective reaction the different species potentially found in solution at the end of the reaction to partition between the organic and aqueous layers during the liquid-liquid extraction step? Explain your prediction. Oxone), how you would expect
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