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Phosphorus oxychloride → HCID 23153703, 화합물

HRID 1990791
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인쇄 미리보기

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HRID 1990791 반응식
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[N:13]=[CH:12][C:11]([C:14]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17](=O)[NH:16][N:15]=2)=[CH:10][CH:9]=1>N1C=CC=CC=1>[Cl:3][C:17]1[C:18]2[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:14]([C:11]2[CH:12]=[N:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=2)=[N:15][N:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 23153686HCID 23153686, 화합물

생성물 1

HCID 23153703HCID 23153703, 화합물수율 55.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
120 °C

실험 절차

932 μl (10 mmol) of phosphorus oxychloride was added to a pyridine solution (5 ml) of 507 mg (2 mmol) of 4-(6-methoxypyridin-3-yl)-2H-phthalazin-1-on, and the reaction liquid was stirred at 120° C. for 30 minutes. This was concentrated under reduced pressure, aqueous saturated sodium hydrogencarbonate solution 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 300 mg (yield: 55%) of 1-chloro-4-(6-methoxypyridin-3-yl)-phthalazine as a brown solid.

후처리

  1. customthe reaction liquid
  2. concentrationThis was concentrated under reduced pressure, aqueous saturated sodium hydrogencarbonate solution
  3. additionwas added to the reaction liquid
  4. extractionextracted with chloroform
  5. washthe organic layer was washed with saturated saline water
  6. dry with materialThis was dried with anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ef8950bffc504662a2211637cbcb3b82
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645756B2

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