反応 #2286303

反応方程式

2-[3,5-dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol

2-[3,5-Dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol

sodium acetate

acetic acid

→

acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester

収率 100.0%

Acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester

収率 100.0%

反応条件

後処理

1. 1
   温度At this time, the reaction mixture was cooled to room temperature
2. 2
   濃縮was concentrated under vacuum
3. 3
   workup.ADDITIONThe resulting residue was diluted with methylene chloride (25 mL)
4. 4
   洗浄was washed with water (10 mL)
5. 5
   その他The organic layer was separated
6. 6
   洗浄was washed with a saturated aqueous sodium bicarbonate solution (10 mL)
7. 7
   抽出extracted with methylene chloride (10 mL)
8. 8
   乾燥dried with sodium sulfate
9. 9
   ろ過filtered
10. 10
    濃縮concentrated
11. 11
    その他dried under high vacuum overnight

実験手順

A solution of 2-[3,5-dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol (17) (500 mg, 1.38 mmol) in glacial acetic acid (5 mL) was treated with sodium acetate (230 mg, 2.8 mmol) and heated to 114° C. for 24 h. At this time, the reaction mixture was cooled to room temperature and was concentrated under vacuum. The resulting residue was diluted with methylene chloride (25 mL) and was washed with water (10 mL). The organic layer was separated and was washed with a saturated aqueous sodium bicarbonate solution (10 mL). The waters layers were combined and extracted with methylene chloride (10 mL). The organic layers were combined and dried with sodium sulfate, filtered, concentrated and dried under high vacuum overnight to afford acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester (34) (531 mg, 100%) as a white solid; LRMS for C17H18Cl2N2O4 (M+) m/z=385 Molecular Weight=385.2500; Exact Mass=384.0644

出典