3-Fluorophenol → 2-(3-Fluorophenoxy)acetamide

HRID 56278

反応式

HRID 56278 の反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.Br[CH2:10][C:11]([NH2:13])=[O:12].C([O-])([O-])=O.[K+].[K+].C([O-])([O-])=O.[Cs+].[Cs+]>CC(C)=O>[F:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:10][C:11]([NH2:13])=[O:12]

参加物

6

反応物 4

HCID 97433-FluorophenolHCID 10796Cesium carbonateHCID 11430Potassium CarbonateHCID 696322-Bromoacetamide

生成物 1

HCID 189381052-(3-Fluorophenoxy)acetamide収率 30%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 3-fluorophenol (11.2 g, 100 mmol), 2-bromoacetamide (13.8 g, 100 mmol), K2CO3 (13.82 g, 100 mmol) and Cs2CO3 (32.58 g, 100 mmol) in acetone (150 mL) was refluxed overnight. The mixture was cooled to rt and filtered and the filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1) to give the title compound as a white solid (5.06 g, 30%).

後処理

  1. temperaturewas refluxed overnight
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated in vacuo
  4. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1)

出典と根拠

ORDレコード
ord-7eb07fbcc8ef449b86ac184e3c4a8ea6
出典データセット
uspto-grants-2016_09
特許番号
US09434695B2

関連ノート

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