반응 #2286342

반응 방정식

N-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-ylsulfanyl)-phenyl]-acetamide

N-[3,5-Dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-ylsulfanyl)-phenyl]-acetamide

sodium hydroxide

→

6-(4-amino-2,6-dichloro-phenyl sulfanyl)-4-isopropyl-2H-pyridazin-3-one

수율 99.1%

6-(4-Amino-2,6-dichloro-phenylsulfanyl)-4-isopropyl-2H-pyridazin-3-one

수율 99.1%

용매

methanol

water

water

반응 조건

후처리

1. 1
   온도The reaction was then heated
2. 2
   온도to reflux for 18 h
3. 3
   추출extracted with ethyl acetate (3×300 mL)
4. 4
   세척The organics were washed with a saturated aqueous sodium chloride solution (1×200 mL)
5. 5
   건조dried with magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated under vacuum

실험 절차

A mixture of N-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-ylsulfanyl)-phenyl]-acetamide (84) (4.0 g, 10.7 mmol) in methanol (15 mL) and water (15 mL) was treated with powdered sodium hydroxide (2.14 g, 53.5 mmol). The reaction was then heated to reflux for 18 h. At this time, the reaction was cooled to 25° C., diluted with water (500 mL) and extracted with ethyl acetate (3×300 mL). The organics were washed with a saturated aqueous sodium chloride solution (1×200 mL), dried with magnesium sulfate, filtered and concentrated under vacuum to afford 6-(4-amino-2,6-dichloro-phenyl sulfanyl)-4-isopropyl-2H-pyridazin-3-one (85) (3.5 g, 99%) as a light tan solid. The material was used without further purification; ES(+)-HRMS m/e calcd for C13H13Cl2N3OS (M+H)+ 330.0229, found 330.0229. Exact Mass=329.0156; Molecular weight=330.24

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