反应详情

To a solution of 8-amino-1-methyl-4,5-dihydro-1H-1,7,9-triaza -cyclopenta[a]naphthalene-3-carboxylic acid ethyl ester M1 (0.51 mmol) in 95% EtOH (10 mL), KOH (1.54 mmol) was added. The mixture was heated to reflux for 10 h then cooled and evaporated to dryness. The residue was dissolved in 30 mL of water, acidified with glacial AcOH and the precipitate was filtered and washed with water. The product was dried affording the title compound (75% yield). ESI (+) MS: m/z 245 (MH+). 1H NMR: 2.65 (t, J=7.80, 2H), 2.92 (t, J=7.80, 2H), 4.15 (s, 3H), 6.39 (bs, 2H), 7.78 (s, 1H), 8.01 (s, 1H), 12.30 (bs, 1H).

1. temperatureThe mixture was heated
2. temperatureto reflux for 10 h
3. temperaturethen cooled
4. customevaporated to dryness
5. dissolutionThe residue was dissolved in 30 mL of water
6. filtrationthe precipitate was filtered
7. washwashed with water
8. customThe product was dried