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29th April 2015 @ 06:49
With Paul King 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] and [blog=8162]Synthesis of 2-Chloro-6-hydrazinylpyrazine (AEW 85-3)[/blog]   2,6-dichloropyrazine (21 g, 141 mmol, 1 eq) was dissolved in EtOH (282 mL, 0.50 M), and hydrazine hydrate (13.5 mL, 270 mmol, 2 eq) added. The reaction mixture was stirred at reflux for 8 hours. The solvent was removed under reduced pressure to give a pale yellow solid. Water (~150 mL) and EtOAc (~200 mL) were added, and the mixture was shaken in an attempt to dissolve all solid. The organic layer was removed, the aqueous layer extracted with EtOAc (3 x 100 mL), and the combined organic layers washed with brine (~30 mL) before being concentrated under reduced pressure to yield a yellow solid  Data: Crude 300 MHz Data: [data]14875[/data][data]14873[/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.zip
AEW 85.pdf