All Notebooks | Help | Support | About
14th August 2013 @ 01:23
AEW 73-1 (80 mg, 0.26 mmol, 1 equiv.) was dissolved in CH2Cl2 (2.6 mL), EDCI (60 mg, 0.31 mmol, 1.2 equiv.) and HOBt (3.5 mg, 0.03 mmol, 0.1 equiv.) were added and the mixture stirred for 20 minutes. Ammnonia (28% aq. soln., 0.24 mL, 0.39 mmol, 1.5 equiv.) was added and the reaction mixture stirred at room temperature. Reaction mixture stirred for 4 hours, still SM. Stirred o/n still SM by TLC. Reaction quenched by addition of an aqueous solution of sodium hydrogen carbonate and then extracted with CH2Cl2, washed with brine, dried (MgSO4), filtered and evaporated to yield a yellow oil with white/yellow crystals. Purified by column using 1-10% MeOH in DCM. Gave desired poduct as white semi-solid (52 mg, 0.17 mmol, 66% yield). Data: TLC 5% MeOH in CH2Cl2 (20 h) [data]7272[/data] 500 MHz [data]15913[/data][data]15917[/data][data]15919[/data] Hazard and Risk Assessment: [data]7272[/data]
Attached Files
AEW 77-1.png
AEW 77-1.pdf
AEW 77-1 5% MeOH in DCM.png
AEW 77-1.zip
AEW 77-1.pdf
AEW 77-1.pdf