1,2-Dimethyl-4-(2-fluoro-4-nitrophenyl)piperazine → HCID 63610994、化合物

HRID 2117624ノート

反応式

HRID 2117624 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][C:9]=2[F:17])[CH2:4][CH:3]1[CH3:18]>[Pd].C(O)C>[NH2:14][C:11]1[CH:12]=[CH:13][C:8]([N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH:3]([CH3:18])[CH2:4]2)=[C:9]([F:17])[CH:10]=1

参加物

4

反応物 1

HCID 692010101,2-Dimethyl-4-(2-fluoro-4-nitrophenyl)piperazine

生成物 1

HCID 63610994HCID 63610994、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒2 回

実験手順

Absolute ethanol (2 mL) was added to a two-necked round-bottomed flask containing palladium on carbon (0.09 g, 0.42 mmol). The reaction vessel was evacuated and purged with nitrogen three times. 1,2-Dimethyl-4-(2-fluoro-4-nitrophenyl)piperazine (1.06 g, 4.2 mmol) in absolute ethanol (10 mL) was added and the vessel purged thrice more with nitrogen. After purging thrice with hydrogen, the reaction was left to stir under a hydrogen atmosphere at room temperature for 18 h. The reaction mixture was filtered through a pad of Celite washing with additional ethanol. Excess ethanol was removed under reduced pressure to afford the title compound as an off-white oil. LC-MS (UV 215nm): 93%; m/z 224.35; 0.58 min.

後処理

  1. customThe reaction vessel was evacuated
  2. custompurged with nitrogen three times
  3. customthe vessel purged thrice more with nitrogen
  4. customAfter purging thrice with hydrogen
  5. waitthe reaction was left
  6. filtrationThe reaction mixture was filtered through a pad of Celite
  7. washwashing with additional ethanol
  8. customExcess ethanol was removed under reduced pressure

出典と根拠

ORDレコード
ord-30d7dd5be29d425887ce6c85a69df762
出典データセット
uspto-grants-2008_10
特許番号
US07442698B2

反応ノート

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