1-Methylpiperazine → 1-[2-(4-Methyl-1-piperazinyl)-6-nitrophenyl]ethanone

HRID 1914753ノート

反応式

HRID 1914753 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=1[C:11](=[O:13])[CH3:12].[CH3:14][N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1>>[CH3:14][N:15]1[CH2:20][CH2:19][N:18]([C:2]2[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=2[C:11](=[O:13])[CH3:12])[CH2:17][CH2:16]1

参加物

3

反応物 2

HCID 531671-MethylpiperazineHCID 204565701-(2-Chloro-6-nitrophenyl)ethan-1-one

生成物 1

HCID 594543161-[2-(4-Methyl-1-piperazinyl)-6-nitrophenyl]ethanone収率 68.9%

反応条件

温度
120 °C

実験手順

In a cylindrical quartz tube were placed 1-(2-chloro-6-nitro-phenyl)-ethanone (300 mg, 1.5 mmol) and N-methyl-piperazine (12 ml, 180 mmol). The reaction was heated for 40 hours at 120° C. The solvent was removed under reduced pressure and the residue was dissolved in DCM. The solution was washed twice with water and the organic phase was dried over anhydrous Na2SO4. The crude was purified by flash chromatography (acetone/MeOH 75:25) affording the desired compound (272 mg, 46% yield), as a yellow solid.

後処理

  1. customIn a cylindrical quartz tube were placed
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in DCM
  4. washThe solution was washed twice with water
  5. dry with materialthe organic phase was dried over anhydrous Na2SO4
  6. customThe crude was purified by flash chromatography (acetone/MeOH 75:25)

出典と根拠

ORDレコード
ord-5aa2c5b36fc14360af46dff00959ba66
出典データセット
uspto-grants-2013_12
特許番号
US08614220B2

反応ノート

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