Reaktion #1244404
ord-22102514dcb14742a2af528a0cd602d7
Reaktionsgleichung
Edukte
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1TemperaturThe reaction mixture was cooled to room temperature
- 2Einengenconcentrated
- 3workup.ADDITIONThe resulting residue was diluted with methylene chloride (200 mL)
- 4Waschenwas washed with water (150 mL)
- 5SonstigeThe organic layer was separated
- 6workup.ADDITIONHexanes (3×200 mL) were added to the residue in portions
- 7Einengensubsequently concentrated under vacuum
- 8workup.ADDITIONThe resulting semi-solid was diluted with a minimum amount of ether
- 9FiltrationThe resulting white solid was filtered
- 10Waschenwashed with cold ether
- 11Sonstigedried under high vacuum overnight
Vorschrift
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