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20th February 2012 @ 22:12
[i]PS = Pictet-Spengler[/i] ======================================= [b][u]Summary and Conclusion[/b][/u] No reaction of the dimethoxy [i]N[/i]-benzoyl PZQ analogue peptide acetal in the presence of silver chloride. ======================================= START: 21/02/12 FINISH: 21/02/12 [b][u]Background[/b][/u] [b][u]Hazard and Risk Assessment[/b][/u] [data]3233[/data] [b][u]Previous Related Experiments[/b][/u] [blog]4376[/blog] [b][u]Following Experiments[/b][/u] [blog]4520[/blog] [b][u]Procedure[/u][/b] MNR10-2 (253.6 mg, 0.553 mmol) was dissolved in toluene (25 mL) before the addition of AgCl (29.1 mg, 0.203, 37 mol%) at rt. The mixture was immediately placed in a pre-heated oil bath at 90 °C and reflux heated from 10:55. Taken off heat after 1 hour. [b]Monitoring the Reaction Progress by TLC[/b] All TLCs were eluted with EtOAc/hexane, 5:3, v/v and stained with KMnO4. [data]3279[/data][data]3283[/data][data]3285[/data][data]3287[/data] [b][u]Summary and Conclusion[/b][/u] No reaction of the dimethoxy [i]N[/i]-benzoyl PZQ analogue peptide acetal in the presence of silver chloride. ----------------------------------------------------------------------------- NOTES 21/02/12 - Suspect the silver has been reduced - Black solid in flask. -----------------------------------------------------------------------------
Attached Files
Hazard and Risk Assessment KAB8-13
Scheme KAB8-13
Table KAB8-13
TLC of reaction mixture (5 min)
Reaction mixture (5 min)
TLC of reaction mixture (15 min)
TLC of reaction mixture (30 min)
TLC of reaction mixture (1 h)