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

HRID 324733

반응식

HRID 324733 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6971f7937fac4e5c91add1eb2a6f7231
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218547B1

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