which nmr is the best and which one is the poor? reason for why it is good or ba
ID: 1041684 • Letter: W
Question
which nmr is the best and which one is the poor? reason for why it is good or bad??
Procedure: Part 1: The Reaction 1. Add 0.300 g of p-nitrobènzaldehyde to an J Add 3 mL 30% KOH with a pipet by allowing it to run a w n the walls of the test tube to wash any powder to the bottom. The mixture will be viscous test tube. Grind with a glass stir rod Cla 2. Stir with a glass stir rod for 15-20 minutes at room temperature 3. Label a centrifuge tube "Acid". Label another centrifuge tube "Alcohol" . 4. Transfer the reaction mixture to the "Acid" tube and add 2mL of DI water and 2mL dichloromethane (DCM). Cap, shake, vent occasionally. Allow layers to separate 5. Transfer organic layer (DCM, bottom layer) to the centrifuge labeled "Alcohol" with a pipet. Extract the AQ layer in "Acid cent. tube with another 2mL of DCM and transfer organic layer to "Alcohol" cent. tube. Wash combined DCM layers in "Alcohol" tube with 2mL DI water and then transfer the organic layer to a clean test tube labeled Alcohol 2". Dry over sodium sulfate for 5 minutes fee Part 2: Isolate/Purify p-nitrobenzoic acid 1. Cool a solution of 2mL methanol and 0.5mL water in an ice bath. Slowly add 3mL of HCl to the AQ layer in the "Acid" tube to precipitate the p R nitrobenz oic acid. Cap the tube and cool in ice bath for 5 minutes. Collect crystal wi Hirsch funnel and wash with waters Transfer crystals (Manual says paper, but our Hirsch funnels have a frit and use no filter paper.) to 50mL E?flask, add to also transfer filtera? pCM 3mL of MeOH, and warm on hot plate until crystals just dissolve. If small amount of solid remains in flask, filter through a cotton plug in a short p into a clean flask. Rinse flask with a little hot methanol and filter through the cotton plugged pipet into the clean flask. Add 1 mL of water. If any crystals form, warm to redissolve. Allow solution to cool to room temperature, and then place in an ice bath. Collect crystals, wash with the cold MeOH/'water solution prepared in Part 2, step, 1. May dry in 100-110°C oven for a few minutes.. Part 3: Isolate/Purify p-nitrobenzyl alcohol 1. Filter the dried solution in "Alcohol 2" through a clean, cotton plugged short pipet, or decant into a clean 50mL E. flask. Use 1 mL of DCM to rinse the drying agent and filter or decant into the E. Flask. Concentrate the DCM to about 1mL by gently blowing a stream of air over the surface. Add 2mL of petroleum ether to precipitate the alcohol 2. Collect the crystals with a Hirsch funnel and wash with 2 mL petroleum ether. Allow to air dry. Do not put in oven. (MP- 92-94°C) Part 4: Mass, %yield, MP, TLC, IR, NMR Spot starting material, and both products using DCM to dissolve. The eluent is 10%MeOH/DCM (stockroom will prepare). Visualize with UV. Take IR of both products (half of class does each, everyone prints 2 copies and trades one with someone) Take NMR of the acid. ang e Waste: DCM, methanol, and petroleum ether disposed of in organic waste bottle Aqueous layer may be washed down the sink with lots of running water Acid 2232-23 2.Explanation / Answer
ANSWER:
The main reasons for this are;
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