Water → β-Amino-3,4-difluorobenzeneethanol

HRID 324312

反応式

HRID 324312 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:9]2[CH2:13][O:12]C(=O)[NH:10]2)[CH:5]=[CH:6][C:7]=1[F:8].O.[OH-].[K+]>C(O)C>[NH2:10][CH:9]([C:4]1[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=1)[CH2:13][OH:12]

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 220487464-(3,4-Difluorophenyl)-1,3-oxazolidin-2-one

生成物 1

HCID 22048878β-Amino-3,4-difluorobenzeneethanol収率 87.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of (+)-4-(3,4-difluorophenyl)-oxazolidin-2-one (1.39 mmol, 0.27 g) in 5.0 mL ethanol was added 5.0 mL of water and pellets of potassium hydroxide (5.0 mmol, 0.28 g). The resulting solution was then heated to reflux overnight. The solvent was removed in vacuo and the resulting residue was extracted with EtOAc (2×50 mL). The organic extracts were washed with brine and the organic layer was dried over Na2SO4. It was filtered and the solvent was removed in vacuo to obtain (+)-2-amino-2-(3,4-difluorophenyl)-ethanol as a white solid (0.21 g, 87% yield).

後処理

  1. temperatureThe resulting solution was then heated
  2. temperatureto reflux overnight
  3. customThe solvent was removed in vacuo
  4. extractionthe resulting residue was extracted with EtOAc (2×50 mL)
  5. washThe organic extracts were washed with brine
  6. dry with materialthe organic layer was dried over Na2SO4
  7. filtrationIt was filtered
  8. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-7a2d0977468b493880692134b500571a
出典データセット
uspto-grants-2001_04
特許番号
US06218390B1

関連ノート

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