Water → 4-Acetyl-n-(3-(1-acetylpiperazin-4-yl)phenyl)-2-nitroaniline

HRID 49816

反応式

HRID 49816 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7](F)=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1)=[O:3].[C:14]([N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:24]=[C:25]([CH:27]=[CH:28][CH:29]=2)[NH2:26])[CH2:19][CH2:18]1)(=[O:16])[CH3:15].O>CN1C(=O)CCC1>[C:2]([C:4]1[CH:9]=[CH:8][C:7]([NH:26][C:25]2[CH:27]=[CH:28][CH:29]=[C:23]([N:20]3[CH2:19][CH2:18][N:17]([C:14](=[O:16])[CH3:15])[CH2:22][CH2:21]3)[CH:24]=2)=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1)(=[O:3])[CH3:1]

参加物

5

反応物 3

HCID 962WaterHCID 27346124'-Fluoro-3'-nitroacetophenoneHCID 111175391-[4-(3-Aminophenyl)piperazin-1-yl]ethan-1-one

生成物 1

HCID 223302264-Acetyl-n-(3-(1-acetylpiperazin-4-yl)phenyl)-2-nitroaniline

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
80 °C

実験手順

A mixture of 1b (0.75 g, 4.1 mmol) and 2d (0.9 g, 4.1 mmol) in anhydrous NMP (2 ml) was heated to 80° C. overnight under a stream of nitrogen. After cooling water (20 ml) was added and the mixture was extracted with dichloromethane. The organic extract was dried over sodium sulfate and the solvent was removed under reduced pressure. The residue was purified by column-chromatography on silica gel using ethyl acetate as the eluent to yield 4-acetyl-N-(3-(1-acetylpiperazin-4-yl)phenyl)-2-nitroaniline as an oil.

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with dichloromethane
  3. extractionThe organic extract
  4. dry with materialwas dried over sodium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified by column-chromatography on silica gel

出典と根拠

ORDレコード
ord-da6a3f7e113d4c7caef77cfec8bc0628
出典データセット
uspto-grants-2004_03
特許番号
US06710044B2

関連ノート

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