Hydroxyamine hydrochloride → 1-(3,4-Difluorophenyl)-2-hydroxy-propan-1-one-oxime

HRID 1275217노트

반응식

HRID 1275217 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:9](=O)[CH:10]([OH:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8].Cl.[NH2:15][OH:16].C([O-])(=O)C.[Na+]>CO>[F:1][C:2]1[CH:3]=[C:4]([C:9](=[N:15][OH:16])[CH:10]([OH:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8]

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 229935141-(3,4-Difluorophenyl)-2-hydroxy-propan-1-one

생성물 1

HCID 740145381-(3,4-Difluorophenyl)-2-hydroxy-propan-1-one-oxime수율 97.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a well stirred solution of 1-(3,4-difluorophenyl)-2-hydroxy-propan-1-one (5.5 g, 29.6 mmol) in MeOH (200 mL) was added hydroxylamine hydrochloride (2.6 g, 38.4 mmol) and sodium acetate (8.1 g, 59.2 mmol) and the the turbid solution was stirred overnight at room temperature. The solvent was evaporated and the residue was extracted with CH2Cl2. The organic layer was washed with sat. NaHCO3, separated, dried over Na2SO4 and then filtered. The solvent was removed in vacuo to obtain 1-(3,4-difluorophenyl)-2-hydroxy-propan-1-one-oxime as an orangish yellow oil (5.8 g, 97%). It was used in the next step without purification.

후처리

  1. customThe solvent was evaporated
  2. extractionthe residue was extracted with CH2Cl2
  3. washThe organic layer was washed with sat. NaHCO3
  4. customseparated
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-6d84e051a360467b8d2d4f0108779ee9
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06159990

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