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Phosphorus oxychloride → 3-Chloro-6-(4-methoxyphenyl)pyridazine

HRID 1990774
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HRID 1990774 반응식
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:19]=[N:18][C:17](O)=[CH:16][CH:15]=2)=[CH:10][CH:9]=1>O>[Cl:3][C:17]1[N:18]=[N:19][C:14]([C:11]2[CH:12]=[CH:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=2)=[CH:15][CH:16]=1
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참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 28101666-(4-Methoxyphenyl)-2,3-dihydropyridazin-3-one

생성물 1

HCID 122575013-Chloro-6-(4-methoxyphenyl)pyridazine수율 40%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

With cooling with ice, 50 ml of phosphorus oxychloride was added to 10.00 g (49.5 mmol) of the obtained 6-(4-methoxyphenyl)-pyridazin-3-ol, and the reaction liquid was stirred under reflux for 6 hours. Water was added to the reaction liquid, extracted with chloroform, and the organic layer was washed with saturated saline water. This was dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain 4.41 g (yield: 40%) of 3-chloro-6-(4-methoxyphenyl)-pyridazine as a white solid.

후처리

  1. customthe reaction liquid
  2. temperatureunder reflux for 6 hours
  3. extractionextracted with chloroform
  4. washthe organic layer was washed with saturated saline water
  5. dry with materialThis was dried with anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-936e47842d8540a98e4314fa99ceaf21
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645756B2

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