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From the procedure 2. Add 20 mL of ethanol and a few boiling chips to the flask 3. Swirl the mixture gently for 5 minutes to allow dissolution and the acid-base reaction to occur. REPORT 4. Attach a water condenser to the round-bottom flask 5. Remember, water goes in the bottom and out the top. Attach a clamp holder to the end of the drain tube to keep it weighted in the drain. Turn water to a trickle. If it is slowly draining, it is high enough. Begin a low flow of water through the condenser. 6. Place the set up on a heating/stir plate. 7. Reflux the solution until all of the solids have dissolved. 8. Remove the condenser and add 1.0 mL of iodoethane to the flask. Volume of iodoethane used (mL) Syringe reading the entire volume is dispensed From the procedure 0.9 0.8 SUMMARY int a gentle boil for 1 hour. 1.0
From the procedure 9. Reflux the mixture at a gentle boil for 1 hour. 10. Set up an ice bath toward the end of the reflux time. 11. After refluxing, remove the heat source and carefully pour the reaction mixture over about 25 g of ice in a 250 ml beaker. 12. Use a few mL of water to rinse the round bottom flask. Add this to the beaker containing the ice and your product. 13. Stir the mixture and gently scratch the bottom and sides of the flask with a stir rod to induce crystallization. 14. Collect the crystals using vacuum filtration. 15. Move the crystals from the funnel to a watch glass for drying and place the watch glass in the oven for about 5 minutes. 16. Measure and record the mass of the crystals. Mass of product obtained (g) Note: The balance was tared with the weigh paper before adding the dry crystals O 1.138 g -0/T- 1.138
(10pts) ¹H NMR Analysis From the procedure 19. Dissolve a small amount (~10 mg) of the product in 700 microliters of CDCl3. place the solution in an NMR tube and obtain a proton NMR spectrum. ¹H NMR Spectrum for Product Obtained 3H 1H 2H (2pts) 1H 5 2H PPM You can download the 'H NMR spectra by clicking here. (2pts) Upload your annotated ¹H NMR spectrum. 2 If you are completing this report virtually, download the 'H NMR spectra above and annotate it. 3H Browse your files to upload or Drag and Drop Max attachments: 5 | Max Size: 20.00MB each
(2pts) Complete the following table to analyze the NMR signals in ppm. Normal : BIU fxi XIX→ BEIT: 1 Report Table NS.2: Proton NMR Analysis Chemical shift, ppm Integration EE Partial Multiplicity structure (2pts) Use three key signals to justify what compound(s) that you think are present. Normal : BI U X₂X¹ fxl BT ili EEE Tx (2pts) Does this suggest that your reaction worked? Use three key signals to justify your answer. Normal : BIU X₁ X² EES BIT Elli T Tx
(2pts) Does this suggest that your reaction worked? Use three key signals to justify your answer. Normal : BIU fx X₁ X² → BEIT & Normal : BIU fx| BIT Ei (2pts) What does this NMR data indicate about the purity of the product? Use three key signals to justify your answer. X₂ X²EBE (1pts) Upload notebook pages (1pts) Upload images of your lab notebook pages. Tx Browse your files to upload or Drag and Drop Max attachments: 10 | Max Size: 20.00MB each Saved Tx