反应详情

A solution of 2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-8-methoxy-4,5-dihydro-6-oxa-1,3a,9-triaza-benzo[e]azulene (1.0 g, 2.97 mmol) in 48% aqueous HBr (5 mL) and acetic acid (5 mL) was heated at 80° C. for 7.5 h before being concentrated in vacuo. The resultant residue was suspended in water (10 mL) and pH adjusted to ˜6 using 5N aqueous NaOH. The precipitate formed was filtered off, washed with water then dried in vacuo to give 2-(2-Isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a,9-triaza-benzo[e]azulen-8-ol as a white solid (1.01 g, 100%). LCMS RT=2.01 min, [M+H]+=327. 1H NMR 400 MHz (DMSO-d) δ: 8.42 (1 H, s), 7.85 (1 H, s), 5.85 (1 H, s), 5.69-5.65 (1 H, m), 4.55-4.54 (2 H, m), 4.50-4.46 (2 H, m), 2.27 (3 H, s), 1.44 (6 H, d, J=6.59 Hz).

1. concentrationbefore being concentrated in vacuo
2. customThe precipitate formed
3. filtrationwas filtered off
4. washwashed with water
5. customthen dried in vacuo