Water → HCID 2915197、化合物

HRID 1282084ノート

反応式

HRID 1282084 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1)(=[O:3])[CH3:2].F[C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[N+:18]([O-:20])=[O:19].C(=O)([O-])[O-].[K+].[K+].O>C(#N)C>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=2[N+:18]([O-:20])=[O:19])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 677672,5-DifluoronitrobenzeneHCID 837951-Acetylpiperazine

生成物 1

HCID 2915197HCID 2915197、化合物収率 86.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 1-acetylpiperazine (20 g) in acetonitrile (50 ml) were added 2,5-difluoronitrobenzene (25 g) and potassium carbonate (22 g) and the mixture was refluxed under heating at room temperature for 4.5 hr. The reaction mixture was poured into water 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 to give the title compound (36 g) as a red solid.

後処理

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

出典と根拠

ORDレコード
ord-9f3b9fcbb6d2486d92c6716417e52ca1
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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