with TLC on silica gel with dimethylformamide (Rf 0.9) or aqueous 80% methanol (Rf 0.8). Attempted recrystallization usually resulted in partial decomposition, as shown by TLC. The analytical sample was dried for 9 h at 0.1 Torr at 100 °C. The compound darkened above 240 °C but did not melt up to 400 °C; 100-MHz !H NMR (Me2SO-d8) 8.55 (s, 1, NCHN), 8.10 (s, 1, CH=CB2), 7.64 (broadened s, 1, NH), 7.18 (broadened s, 1, NH), 3.42 (s, ~10, NH, BOH, and H20 from solvent); on addition of methanol dropwise, the 7.64 peak broadened, shifted downfield, and disappeared, and the 7.18 peak broadened somewhat without shifting; NMR (CD3OD)8.31 (brd s.
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