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31st October 2013 @ 10:19
Repeat of [blog=7972]Synthesis of 2-Chloro-6-hydrazinylpyrazine (AEW 85-1)[/blog], see also [blog=8025]Synthesis of 2-Chloro-6-hydrazinylpyrazine (AEW 85-2)[/blog] Started 8.30 am  2,6-Dichloropyrazine (4 g, 27.0 mmol) was vigorously stirred in ethanol (40 mL) and hydrazine hydrate (1.32 mL, 1.36 g, 27.0 mmol) was added. The resulting mixture was heated at 80 ˚C for 12 h. Reaction incomplete. Stirred overnight and still SM. Stirred over the weekend..with a TLC check...couldn't see SM. Solvent evaporated - still SM by NMR. Resubmitted to the reaction conditions.   Data: 1H NMR (200 MHz, CDCl3): incomplete  [data]7951[/data][data]7949[/data] 1H NMR (300 MHz, CDCl3):  [data]7945[/data][data]7947[/data] Hazard and Risk Assessment: See [blog=7972]Synthesis of 2-Chloro-6-hydrazinylpyrazine (AEW 85-1)[/blog] InChi Strings: InChI=1S/C4H2Cl2N2/c5-3-1-7-2-4(6)8-3/h1-2H to InChI=1S/C4H5ClN4/c5-3-1-7-2-4(8-3)9-6/h1-2H,6H2,(H,8,9)  
Attached Files
AEW 85-3.pdf
AEW 85-3 200 mhz incomplete.pdf