تفاعل #2286296
ord-80bff88c65254ce1b1b9e2da6630f0cc
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1درجة الحرارةThe reaction mixture was cooled to room temperature
- 2تركيزconcentrated
- 3workup.ADDITIONThe resulting residue was diluted with methylene chloride (200 mL)
- 4غسيلwas washed with water (150 mL)
- 5أخرىThe organic layer was separated
- 6workup.ADDITIONHexanes (3×200 mL) were added to the residue in portions
- 7تركيزsubsequently concentrated under vacuum
- 8workup.ADDITIONThe resulting semi-solid was diluted with a minimum amount of ether
- 9ترشيحThe resulting white solid was filtered
- 10غسيلwashed with cold ether
- 11أخرىdried under high vacuum overnight
الإجراء التجريبي
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