Why do you think a large excess of sulfolene was used? This is the expermimnet: Mix 2.5 g of sulfolene, 5 mL of xylene, and 1.25 g of maleic anhydride in a 50 mL round bottom flask. Fit the flask with a water‐cooled reflux condenser. Heat the contents of the flask using the thermowell (make sure the round‐ bottom flask is NOT touching the heating mantle) until the xylene begins to gently reflux, and then maintain the reflux for 45 minutes. Periodically check your reflux to ensure the solution is continually boiling and that the reflux ring is lower than the middle of the condenser. Once the reaction mixture has refluxed for 45 minutes, turn off and lower the thermowell, allowing the flask and solution to cool to room temperature. After the flask has reached room temperature (generally about 5‐10 minutes of cooling), cool in an ice bath. Collect the crude product by vacuum filtration. To purify the crude product, recrystallize in 2:1 v/v1 xylene : hexane. How much solvent should you use? Wash the crystals with hexane and allow the recrystallized product to air dry in the funnel for 10 minutes. Weigh your product and then record an IR spectrum of your final product, making sure to label the relevant peaks. Finally, record the melting point of your product and, if you need additional data about the purity of your isolated product, run a TLC with your product and maleic anhydride (don’t forget a co‐spot) in 5% acetic acid, 95% ethyl acetate.
Why do you think a large excess of sulfolene was used?
This is the expermimnet:
Mix 2.5 g of sulfolene, 5 mL of xylene, and 1.25 g of maleic anhydride in a 50 mL round bottom flask. Fit the flask with a water‐cooled reflux condenser. Heat the contents of the flask using the thermowell (make sure the round‐ bottom flask is NOT touching the heating mantle) until the xylene begins to gently reflux, and then maintain the reflux for 45 minutes. Periodically check your reflux to ensure the solution is continually boiling and that the reflux ring is lower than the middle of the condenser. Once the reaction mixture has refluxed for 45 minutes, turn off and lower the thermowell, allowing the flask and solution to cool to room temperature. After the flask has reached room temperature (generally about 5‐10 minutes of cooling), cool in an ice bath. Collect the crude product by vacuum filtration.
To purify the crude product, recrystallize in 2:1 v/v1 xylene : hexane. How much solvent should you use? Wash the crystals with hexane and allow the recrystallized product to air dry in the funnel for 10 minutes.
Weigh your product and then record an IR spectrum of your final product, making sure to label the relevant peaks. Finally, record the melting point of your product and, if you need additional data about the purity of your isolated product, run a TLC with your product and maleic anhydride (don’t forget a co‐spot) in 5% acetic acid, 95% ethyl acetate.
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