Acetic Acid → 4,6-Dichloropyridazin-3(2H)-one

HRID 68459

반응식

HRID 68459 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[Cl:8].C(O)(=[O:12])C>>[Cl:8][C:7]1[C:2](=[O:12])[NH:3][N:4]=[C:5]([Cl:9])[CH:6]=1

참가 물질

3

반응물 2

HCID 176Acetic AcidHCID 951233,4,6-Trichloropyridazine

생성물 1

HCID 580162054,6-Dichloropyridazin-3(2H)-one

실험 절차

3,4,6-Trichloro-pyridazine (34.39 g, 187.5 mmol) in 100 mL acetic acid was heated at reflux for three hours. The resulting mixture was cooled to room temperature and filtered. The filtrate was diluted with ethylacetate. This was washed three times with water, washed with brine, dried over anhydrous MgSO4, concentrated in vacuo, and purified by flash chromatography (30% ethylacetate/hexanes) to yield 4,6-Dichloro-2H-pyridazin-3-one (6.143 g, 37.23 mmol). MS (ESI) 165.0 (M+H)+.

후처리

  1. temperatureat reflux for three hours
  2. filtrationfiltered
  3. additionThe filtrate was diluted with ethylacetate
  4. washThis was washed three times with water
  5. washwashed with brine
  6. dry with materialdried over anhydrous MgSO4
  7. concentrationconcentrated in vacuo
  8. custompurified by flash chromatography (30% ethylacetate/hexanes)

출처 및 근거

ORD 기록
ord-60a5d0ce5d514d2c817804be1c5d4df8
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822457B2

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