1-Methylpiperazine → 1-Methyl-4-(4-methyl-3-nitrophenyl)piperazine

HRID 1907440ノート

反応式

HRID 1907440 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[CH3:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>>[CH3:12][N:13]1[CH2:18][CH2:17][N:16]([C:2]2[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=2)[CH2:15][CH2:14]1

参加物

3

反応物 2

HCID 531671-MethylpiperazineHCID 679654-Fluoro-2-nitrotoluene

生成物 1

HCID 581716321-Methyl-4-(4-methyl-3-nitrophenyl)piperazine収率 48.3%

反応条件

温度
200 °C

実験手順

In a cylindrical quartz tube were placed 4-fluoro-1-methyl-2-nitro-benzene (20.0 g, 129 mmol) and N-methyl-piperazine (26 g, 258 mmol). The reaction was heated for 48 hours at 200° C. until HPLC revealed the disappearance of the starting material. 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 and the solvent was removed under reduced pressure. The final compound (14.65 g, 48% yield) was obtained as a brown oil.

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 solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-a93557995aac4e9bacc2228476afc19f
出典データセット
uspto-grants-2013_12
特許番号
US08598172B2

反応ノート

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