Water → HCID 68707820, compound

Participants

Reaction Steps

To a solution of 1-methyl-1,6-dihydro-1,6,7-triaza-as-indacene-2-carboxylic acid D2 (0.46 mmol) in dry acetonitrile (6 mL) and triethylamine (0.13 mL), first TBTU (2 eq) and, after 10 min, 30% aq ammonium hydroxide solution (2 eq) were added under stirring at rt. After 2 h at rt, the mixture was poured into water and the slurry was extracted with AcOEt. The organic layer was washed with brine, dried (Na2SO4) and concentrated to yield a crude product that was purified by chromatography on silica gel (eluant: MeOH/DCM 1:9). Obtained the title compound (10%). ESI (+) MS: m/z 215 (MH+). 1H NMR: 4.36 (s, 3H), 6.95 (bs, 2H), 7.29 (s, 1H), 7.31 (d, J=8.73, 1H), 7.58 (d, J=8.73, 1H), 8.73 (s, 1H), 13.32 (s, 1H).

Provenance & Evidence