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

HRID 1167713노트

반응식

HRID 1167713 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 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-b8a170e9cd9b486080fc44f774235103
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620815B1

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