I have attached an example and instructions as well as my data. 1. NMR Analysis
Did you successfully synthesize the target compound? Did you successfully purify the product via recrystallization? Discuss your NMR data to prove formation of the product and to indicate success of the purification via recrystallization. Be sure to include chemical shifts, integration values, and splitting patterns along with justifications for aromatic proton chemicals (EDG/EWG). Review the video posted on Canvas for help with annotating the NMR spectrum, but remember that it uses a 300 MHz spectrum instead of a 60/80 MHz spectrum! Does the experimental data match the NMR predictions? If not, how do the chemical shifts, splitting patterns, etc. deviate from your predictions? How does the NMR prove conversion of the starting material to the product? Is there any evidence in the NMR of leftover starting material that proves recrystallization success/failure Please refer to the NMR checksheet on your postlab assignment to compare the starting material to the product. Also discuss any other impurities present (starting material, reagents, solvents, etc). Why are they there?
Think/write in the style of claim, evidence, reasoning to help with you discussion! Use your feedback on previous mini report for guidance!
2 IR Analysis
Did you successfully synthesize the target compound? Did you successfully purify the product via recrystallization? Discuss your IR data to prove formation of the product and to indicate success of the purification via recrystallization. Be sure to include stretching frequencies and what functional group they belong to. How does the IR prove conversion of the starting material to the product? Is there any clear evidence in the IR of leftover starting material? Please refer to your IR checksheet on your postlab assignment to compare the starting material to the product. Any impurities you observed on your NMR should also be labelled and discussed in the IR data (except acetone – that came from cleaning your NMR tube). Think in the style of claim, evidence, reasoning to help with you discussion!
3. Conclusions
Start this paragraph with “In conclusion, the synthesis of 3-chloro-4’-methoxychalcone via Claisen-Schmid Condensation and subsequent purification by recrystallization was successful/unsuccessful…..” Success can be evaluated as synthesis of product, purity, and/or yield. Use general trends seen in your NMR/IR/MP data to support this statement. Tie all pieces of data together (recrystallization purification observations, melting point, physical appearance, yield, NMR/IR data, etc.) in a few sentences. What was the take-home message of this experiment? Were there any major sources of error? What are some thoughtful and scientific improvements for this experiment? Remember, human error should NOT be proposed as a major error or area of improvement. Think about the reaction itself and how the chemistry, monitoring, work-up, and purification could be improved.
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