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12th April 2011 @ 02:06
Experiments on the oxidation of PZQamine to the enamide/imine by molten sulfur. See related experiments on rac-PZQ: [url=http://www.thesynapticleap.org/node/291]Sulfur melt data smogasbord[/url] [data=size:500x180]1041[/data] [b]Hazard and Risk Assessment:[/b] [data]1043[/data] Start time: 11:30 AM 12/04/2011 [b]MW57-1:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (40 mg, 198 µmol, M.W. 202.3 g/mol) and sulfur (12.7 mg, 2 eq., M.W. 32.1 g/mol) were heated at 180°C for 5 min. [b]MW57-2:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (40 mg, 198 µmol, M.W. 202.3 g/mol) and sulfur (12.7 mg, 2 eq., M.W. 32.1 g/mol) were heated at 180°C for 10 min. [data]1045[/data] [b]MW57-3:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (40 mg, 198 µmol, M.W. 202.3 g/mol) and sulfur (12.7 mg, 2 eq., M.W. 32.1 g/mol) were heated at 180°C for 15 min. [data]1160[/data][data]1162[/data][data]1047[/data] Start time: 11:30 AM 12/04/2011 [b]MW57-4:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (20 mg, 99 µmol, M.W. 202.3 g/mol) and sulfur (6.4 mg, 2 eq., M.W. 32.1 g/mol) were heated at 180°C for 30 min. [b]MW57-5:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (20 mg, 99 µmol, M.W. 202.3 g/mol) and sulfur (6.4 mg, 2 eq., M.W. 32.1 g/mol) were heated at 180°C for 1 h. [b]MW57-6:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (20 mg, 99 µmol, M.W. 202.3 g/mol) and sulfur (12.7 mg, 4 eq., M.W. 32.1 g/mol) were heated at 180°C for 15 min. [b]MW57-7:[/b] [url=http://www.ourexperiment.org/racres_pzq/1521][i]rac[/i]-PZQamine[/url] (20 mg, 99 µmol, M.W. 202.3 g/mol) and sulfur (12.7 mg, 4 eq., M.W. 32.1 g/mol) were heated at 180°C for 30 min. [b]References:[/b] [url=http://onlinelibrary.wiley.com/doi/10.1002/ardp.19893221104/abstract][1] Spectral and Chemical Properties of Pyrazino-[2,1-a]-isoquinolin-4-one Derivatives, K. Kiec'-Kononowicz, [i]Arch. Pharm.[/i] [b]1989[/b], [i]322[/i],795-799. DOI: 10.1002/ardp.19893221104.[/url]
Attached Files
Scheme MW57.png
HRAF MW57.pdf
1H NMR MW57-2.pdf
1H NMR MW57-3.pdf
TLC57-3.jpg
TLC57-3a.jpg
TLC57-3a.jpg