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20th August 2013 @ 06:07
Attempted synthesis of side chain in greater purity. See also   13 μL of conc. HCl was added to a suspension of glycolic acid (1.0 g, 13.2 mmol, 1 equiv.) in 3,4-dihydro-2H-pyran (3.6 mL, 39 mmol, 3 equiv.) and the reaction mixture was heated to 80 ˚C  for 30 minutes. Volatiles were evaporated, and the resulting residue was purified by flash column chromatography over silica (Ethyl acetate/Petrol 3:7). Two major fractions collected - very streaky TLC plates with elution of all spots. I think that the material deteriorated on storage in the fridge - should have purified immediately. Second fraction cleaner than first - to be used in next reaction AEW 84-1. http://www.jbc.org/content/276/45/41638.full.pdf+html Data: 1H NMR: Fraction A: [data]7339[/data] Fraction B: [data]7341[/data][data]7343[/data] Hazard and Risk Assessment: [data]7292[/data]
Attached Files
AEW 81-1.png
AEW 81-1 HIRAC.pdf
AEW 81-1-A proton.pdf
AEW 81-1-B proton.pdf
AE 81-1-B impure Carbon.pdf
AEW 81-1-A.zip
AEW 81-1-B.zip