反应详情

Lithium hydroxide monohydrate (9.3 mg, 0.22 mmol) and water (0.19 mL) were added to 1-(1-oxo-1,2,7,8,9,10-hexahydro-benzo[f]quinazolin-3-yl)-1H-pyrazole-4-carboxylic acid ethyl ester (25.0 mg, 73.9 pmol) in THF (0.28 mL). The reaction mixture was stirred at room temperature for 18 h and was then concentrated. The residue was redissolved in water (3 mL) and this solution was brought to pH 1 with 1M aqueous HCl. The resulting precipitate was collected and dried to yield the titled compound (19.6 mg, 85% yield). MS (ESI/Cl): mass calcd. for C16H14N4O3, 310.1; m/z found, 311.1 [M+H]+. 1H NMR (400 MHz, DMSO-d6): 12.98 (s, 1H), 12.42 (s, 1H), 8.92 (s, 1H), 8.23 (s, 1H), 7.51 (d, J=8.5 Hz, 1H), 7.41 (d, J=8.3 Hz, 1H), 3.37 (t, J=5.8 Hz, 2H), 2.83 (t, J=5.3 Hz, 2H), 1.84-1.67 (m, 4H).

1. concentrationwas then concentrated
2. dissolutionThe residue was redissolved in water (3 mL)
3. customThe resulting precipitate was collected
4. customdried