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28th September 2011 @ 01:44
Hazard and Risk Assessment:[data]1430[/data] Procedure:MNR8-1 (80 mg, 0.22 mmol) was stirred with methanesulfonic acid (1.4 mL, 22 mmol) at 60°C and after 3 hours (first TLC) all the starting material had been consumed. The reaction was quenched with saturated sodium carbonate and extracted with EtOAc (20 mL x2). The organic fractions were dried over magnesium sulfate, filtered and concentrated under reduced pressure. Crude proton NMR showed what looked like product and the loss of key starting material peaks. [data]1470[/data] FCC EtOAc/Hexane (50-80%). Frac 27-28:- 0.037 g, 0.1 mmol, 58 % as a white gummy oil. [data]1472[/data][data]1915[/data]   IR [data]5359[/data] Lab book page complete, MNR
Attached Files
MNR11-1 scheme.png
MNR11-1 table.PNG
kab1-2 1H 500.pdf
kab1-2 13C 500.pdf
1b rac IR MNR11-1.jpg