Phosphorus oxychloride → 3-Chloro-5-(3-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine

HRID 1678395ノート

反応式

HRID 1678395 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:13]([CH3:14])=[N:12][NH:11][C:10](=O)[C:9]=2[C:16]2[C:21]([F:22])=[CH:20][C:19]([F:23])=[CH:18][C:17]=2[F:24])[CH:5]=[CH:6][CH:7]=1.P(Cl)(Cl)([Cl:27])=O>>[Cl:27][C:10]1[N:11]=[N:12][C:13]([CH3:14])=[C:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)[C:9]=1[C:16]1[C:21]([F:22])=[CH:20][C:19]([F:23])=[CH:18][C:17]=1[F:24]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 577939355-(3-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one

生成物 1

HCID 577938923-Chloro-5-(3-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine収率 97%

反応条件

温度
110 °C

実験手順

2.34 g of 5-(3-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one and 10 g of phosphorus oxychloride were mixed and stirred at 110° C. for 1 hour. The reaction mixture was allowed to cool down to room temperature and concentrated under reduced pressure. To the residue was added ethyl acetate and ice water, and was separated to two layer. The organic layer was washed sequentially with water and saturated brine, and dried over anhydrous sodium sulfate, then, concentrated under reduced pressure, to obtain 2.39 g of 3-chloro-5-(3-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine (hereinafter, referred to as compound (xx) of the present invention).

後処理

  1. temperatureto cool down to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue was added ethyl acetate and ice water
  4. customwas separated to two layer
  5. washThe organic layer was washed sequentially with water and saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-abb3c412c8854fecba38d964caab0e0c
出典データセット
uspto-grants-2011_08
特許番号
US08008512B2

反応ノート

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