Sodium Hydroxide → 1-(4-Fluoro-2-nitrophenyl)piperazine

HRID 1282079ノート

反応式

HRID 1282079 の反応式
C([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=2[N+:17]([O-:19])=[O:18])[CH2:6][CH2:5]1)(=O)C.[OH-].[Na+]>Cl>[F:16][C:13]1[CH:14]=[CH:15][C:10]([N:7]2[CH2:6][CH2:5][NH:4][CH2:9][CH2:8]2)=[C:11]([N+:17]([O-:19])=[O:18])[CH:12]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 2915197HCID 2915197、化合物

生成物 1

HCID 27374351-(4-Fluoro-2-nitrophenyl)piperazine収率 66.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To 1-acetyl-4-(4-fluoro-2-nitrophenyl)piperazine (10 g) was added 1.2N hydrochloric acid (190 ml) and the mixture was refluxed under heating for 17 hr. The reaction mixture was made alkaline (pH 12) with an aqueous sodium hydroxide solution and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated to give a red oil. The oil was crystallized from ethyl acetate-isopropyl ether-hexane to give the title compound (5.6 g) as a red solid.

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 17 hr
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated
  7. customto give a red oil
  8. customThe oil was crystallized from ethyl acetate-isopropyl ether-hexane

出典と根拠

ORDレコード
ord-2b517e05e2e947339ea6c7fc6614b671
出典データセット
uspto-grants-2002_09
特許番号
US06455528B1

反応ノート

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