Phosphorus oxychloride → Methyl 4-chloro-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylate

HRID 422786

反応式

HRID 422786 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:10](O)=[CH:9][C:8](=[O:12])[N:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:6]=1)=[O:4].P(Cl)(Cl)([Cl:21])=O>>[CH3:1][O:2][C:3]([C:5]1[C:10]([Cl:21])=[CH:9][C:8](=[O:12])[N:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:6]=1)=[O:4]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 54686161Methyl 1,6-dihydro-4-hydroxy-6-oxo-1-phenyl-3-pyridazinecarboxylate

生成物 1

HCID 2784479Methyl 4-chloro-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylate収率 84%

反応条件

温度
85 °C

実験手順

A mixture of 4-hydroxy-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylic acid methyl ester (3.83 g, 15.6 mmol) and phosphorous oxychloride (50 mL) was heated to 85° C. After 20 hours, the reaction mixture was concentrated under reduced pressure. The resulting residue was quenched with water. The precipitate was filtered and dissolved in EtOAc, dried (MgSO4) and concentrated under reduced pressure to yield 3.44 g (84%) of desired product.

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe resulting residue was quenched with water
  3. filtrationThe precipitate was filtered
  4. dissolutiondissolved in EtOAc
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b7dcb8b87bee46558719d3dedc6aa462
出典データセット
uspto-grants-2012_01
特許番号
US08101639B2

関連ノート

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