Sodium Carbonate → 1-(4-Amino-2-fluoro-phenyl)-piperidin-4-one

HRID 895126ノート

反応式

HRID 895126 の反応式
[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[N:11]1[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1.C(=O)([O-])[O-].[Na+].[Na+]>Cl.C(OCC)(=O)C.[Fe]>[NH2:8][C:6]1[CH:5]=[CH:4][C:3]([N:11]2[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]2)=[C:2]([F:1])[CH:7]=1

参加物

6

反応物 2

HCID 10340Sodium CarbonateHCID 37637811-(2-Fluoro-4-nitrophenyl)piperidin-4-one

生成物 1

HCID 223856071-(4-Amino-2-fluoro-phenyl)-piperidin-4-one

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 313Hydrochloric Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Iron powder (16.4 g, 294 mmol) was slowly added to an ice-cold solution of 1-(2-fluoro-4-nitro-phenyl)-piperidin-4-one (7 g, 29.4 mmol), obtained in Preparation 5, in ethanolic HCl (50 ml) at 0° C. and stirred at the same temperature for 2 h. The reaction mixture was basified by the addition of sodium carbonate and pH of the solution was brought to 8. It was then diluted with ethyl acetate (100 ml) and the aqueous layer was separated. The aqueous layer was further extracted with ethyl acetate (100 ml×2). Combined organic extract was washed with water followed by brine and dried over sodium sulfate. Removal of volatiles left a pasty mass (7 g), which was used for the next step.

後処理

  1. customthe aqueous layer was separated
  2. extractionThe aqueous layer was further extracted with ethyl acetate (100 ml×2)
  3. extractionCombined organic extract
  4. washwas washed with water
  5. dry with materialdried over sodium sulfate
  6. customRemoval of volatiles
  7. waitleft a pasty mass (7 g), which

出典と根拠

ORDレコード
ord-cfbf24ad9f084e0e857a029833035daf
出典データセット
uspto-grants-2005_07
特許番号
US06914058B2

反応ノート

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