반응 #2286303

반응 방정식

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

수율 100.0%

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

수율 100.0%

반응 조건

후처리

1. 1
   온도At this time, the reaction mixture was cooled to room temperature
2. 2
   농축was concentrated under vacuum
3. 3
   workup.ADDITIONThe resulting residue was diluted with methylene chloride (25 mL)
4. 4
   세척was washed with water (10 mL)
5. 5
   기타The organic layer was separated
6. 6
   세척was washed with a saturated aqueous sodium bicarbonate solution (10 mL)
7. 7
   추출extracted with methylene chloride (10 mL)
8. 8
   건조dried with sodium sulfate
9. 9
   여과filtered
10. 10
    농축concentrated
11. 11
    기타dried under high vacuum overnight

실험 절차

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

출처