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

HRID 245526노트

반응식

HRID 245526 반응식
[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]

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 46311128Methyl 3,4-difluoro-2-hydroxybenzoate2회

생성물 1

HCID 866581193,4-difluoro-N,2-dihydroxybenzamide수율 101.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2613f28fac264875a25302a439afe995
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658641B2

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