Hydroxylamine → 3,4-difluoro-N,2-dihydroxybenzamide

HRID 577986ノート

反応式

HRID 577986 の反応式
[NH2:1][OH:2].[F:3][C:4]1[C:5]([OH:15])=[C:6]([CH:11]=[CH:12][C:13]=1[F:14])[C:7](OC)=[O:8]>O1CCOCC1>[F:3][C:4]1[C:5]([OH:15])=[C:6]([CH:11]=[CH:12][C:13]=1[F:14])[C:7]([NH:1][OH:2])=[O:8]

参加物

4

反応物 2

HCID 787HydroxylamineHCID 46311128Methyl 3,4-difluoro-2-hydroxybenzoate2 回

生成物 1

HCID 866581193,4-difluoro-N,2-dihydroxybenzamide収率 101.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of hydroxylamine (50% in water) (50 ml, 816 mmol) was added to a solution of methyl 3,4-difluoro-2-hydroxybenzoate (7.75 g, 41.2 mmol) (Intermediate 526) in dioxane (200 ml) and the mixture was stirred at room temperature for 3 days. The mixture was partitioned between water and EtOAc. The aqueous layer was acidified with concentrated HCl and extracted with EtOAc twice more. The EtOAc layers were washed with brine, combined and concentrated to give 7.9 g of a solid.

後処理

  1. customThe mixture was partitioned between water and EtOAc
  2. extractionextracted with EtOAc twice more
  3. washThe EtOAc layers were washed with brine
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-d94324e9b1f64a219fdc60f3215bc250
出典データセット
uspto-grants-2015_05
特許番号
US09040528B2

反応ノート

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