Water → HCID 86651541, compound

Participants

Reaction Steps

4-(2,4-dimethoxybenzyl)-2-{4-[(methylamino)methyl]phenyl}-3,4-dihydro-5H-1,4,8b-triazaacenaphthylen-5-one was dissolved in TFA:H2O:TIPS=8.0:1.5:0.5 (0.1 M) and heated to 120° C. for 30 min at microwave apparatus. The solvent was reduced in vacuo and the crude was purified by reverse phase HPLC (column: C18), using H2O (+0.1% TFA) and MeCN (+0.1% TFA) as eluents, the desired fractions were lyophilized to yield (15% over two steps) the title compound. 1H NMR (400 MHz, DMSO-d6, 300K) δ 8.76 (1H, bs), 8.68 (1H, s) 7.86 (2H, d, J=8.0 Hz), 7.68 (1H, d, J=9.0 Hz), 7.57 (2H, d, J=8.0 Hz), 7.37 (1H, d, J=7.0 Hz), 7.30 (1H, dd, J=9.0, 7.0 Hz), 5.28 (2H, s), 4.17 (2H, s), 2.60 (3H, s). MS (ES+) C17H16N4O requires: 292, found: 293 (M+H)+.

Provenance & Evidence