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24th October 2012 @ 03:52
Product obtained in 64% yield. === Hydrolysis of PMY 58-2 methyl ester to the acid using aqueous sodium hydroxide. [b]Reaction Start Time: 12.30 24/10/12[/b] PMY 58-3 (240 mg, 0.76 mmol, 1 equiv.) was dissolved in hot methanol (15 mL). 5M NaOH(aq) (4 mL) was added and the reaction stirred at room temperature. After 2 hours, reaction not complete. 3 pellets of NaOH added and the mixture heated to reflux briefly then cooled. After 30 minutes, reaction complete. The mixture was acidified using 6M HCl and cooled in a salt/ice bath. Pale yellow needle crystals form. Filtered and washed with water then dried (146 mg, 64%). [b]TLC (5% MeOH/DCM) visualised with UV and vanillin:[/b] [data]3586[/data] [b]NMR:[/b] [data]3702[/data] [b]See also:[/b] [blog]4991[/blog] [blog]3922[/blog] [b]Risk and Hazard Assessment:[/b] As for [blog]488[/blog]
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TLC
1H NMR
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