1,2-Dimethyl-4-(2-fluoro-4-nitrophenyl)piperazine → HCID 63610994, 화합물

HRID 2117624노트

반응식

HRID 2117624 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 63610994HCID 63610994, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-30d7dd5be29d425887ce6c85a69df762
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07442698B2

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