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

HRID 68459

反応式

HRID 68459 の反応式
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

参加物

3

反応物 2

HCID 176Acetic AcidHCID 951233,4,6-Trichloropyridazine

生成物 1

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

実験手順

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)+.

後処理

  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)

出典と根拠

ORDレコード
ord-60a5d0ce5d514d2c817804be1c5d4df8
出典データセット
uspto-grants-2014_09
特許番号
US08822457B2

関連ノート

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