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19th June 2013 @ 03:27
See also: [blog=1795]Deprotection of Boc-Gly-4-aminoantipyrine (PMY 30-3)[/blog], no TFA used at outset as PMY found 4M HCl to be more effective. Procedure: Crude AEW 63-1 was dissolved in THF (6 mL). Yellow solution. HCl (4M in dioxane, 3 mL, 12 mmol) was added dropwise - reaction mixture turned red - stirred at room temperature for 3 hours. Still SM. Reaction mixture stirred overnight - still SM and a yellow slurry had formed which wasn't stirring properly. HCl (4M in dioxane, 2 mL, 8 mmol) was added and the reaction mixture stirred at room temperature for a further 4 hours. Reaction complete. Concentrated to a yellow solution and used directly in AEW 65-1.   Data: TLC (10% MeOH in CH2Cl2) after 19 hours [data]6572[/data]  [data]6588[/data]  [data]16535[/data] Hazard and Risk Assessment: See: [blog=1795]Deprotection of Boc-Gly-4-aminoantipyrine (PMY 30-3)[/blog]
Attached Files
AEW 64-1.png
AEW 64-1.png
AEW 64-1 (10% MeOH in DCM).png
AEW 64-1 after