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Water → 3-Iodo-6-methoxypyridazine

HRID 1378970
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HRID 1378970 반응식
[I:1][C:2]1[N:3]=[N:4][C:5](I)=[CH:6][CH:7]=1.[CH3:9][O-:10].[Na+].O>CO>[CH3:9][O:10][C:5]1[N:4]=[N:3][C:2]([I:1])=[CH:7][CH:6]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 2503833,6-DiiodopyridazineHCID 10942334Sodium Methoxide

생성물 1

HCID 2510323-Iodo-6-methoxypyridazine수율 86%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To 2.73 g (8.23 mmol) of 3,6-diiodopyridazine were added 80 ml of methanol and 3.17 g (16.46 mmol) of 28 wt % of sodium methylate in methanol, and the mixture was stirred at room temperature for 13 hours. Water was added to the reaction mixture, and the solution was extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The obtained crude product was purified by silica-gel column chromatography (200 ml of silica gel, hexane:ethyl acetate=8:1) to give 1.661 g (7.04 mmol) of 3-methoxy-6-iodopyridazine (yield: 86%).

후처리

  1. extractionthe solution was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with a saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe obtained crude product
  6. customwas purified by silica-gel column chromatography (200 ml of silica gel, hexane:ethyl acetate=8:1)

출처 및 근거

ORD 기록
ord-f59764e9804d4fd486ac6fa0a785efe1
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05670492

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