反应详情

温度

125 °C

A mixture of glacial acetic acid (200 mL), sodium acetate (6.1 g, 74.4 mmol) and [3,5-dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-acetic acid (18) (8.3 g, 21.96 mmol) was heated to 125° C. for 24 h. The reaction mixture was cooled to room temperature and concentrated. The resulting residue was diluted with methylene chloride (200 mL) and was washed with water (150 mL). The organic layer was separated. Hexanes (3×200 mL) were added to the residue in portions and then subsequently concentrated under vacuum. The resulting semi-solid was diluted with a minimum amount of ether, scratched, and slurried. The resulting white solid was filtered, washed with cold ether and dried under high vacuum overnight to afford [3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-acetic acid (19) (5.1 g, 65%) as a white solid; LRMS for C15H14Cl2N2O4 (M+) m/z=357. Molecular Weight=357.1958; Exact Mass=356.0331

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated
3. additionThe resulting residue was diluted with methylene chloride (200 mL)
4. washwas washed with water (150 mL)
5. customThe organic layer was separated
6. additionHexanes (3×200 mL) were added to the residue in portions
7. concentrationsubsequently concentrated under vacuum
8. additionThe resulting semi-solid was diluted with a minimum amount of ether
9. filtrationThe resulting white solid was filtered
10. washwashed with cold ether
11. customdried under high vacuum overnight