1-Methylpiperazine → 1-(2-Fluoro-4-nitrophenyl)-4-methylpiperazine

HRID 10774

반응식

HRID 10774 반응식
[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1F.[CH3:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>C(#N)C>[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[N:16]1[CH2:17][CH2:18][N:13]([CH3:12])[CH2:14][CH2:15]1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 1230531,2-Difluoro-4-nitrobenzene

생성물 1

HCID 27830541-(2-Fluoro-4-nitrophenyl)-4-methylpiperazine수율 97%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 3,4-difluoronitrobenzene (12.00 g, 75.4 mmol) (Aldrich) and N-methylpiperazine (18.89 g, 188.6 mmol) in acetonitrile (150 mL) was heated at reflux for 3 h. The reaction mixture was allowed to stand overnight at room temperature, then the solvent was evaporated under reduced pressure and the residue was partitioned between water and ethyl acetate (200 mL each). The aqueous layer was extracted with ethyl acetate (3×200 mL) and the combined organic layers were then washed with water and brine (200 mL each), dried (MgSO4), filtered, and evaporated under reduced pressure to give 1-(2-fluoro-4-nitrophenyl)-4-methylpiperazine as a pale brown solid (17.5 g, 97%, mp 68–70° C.).

후처리

  1. temperatureat reflux for 3 h
  2. customthe solvent was evaporated under reduced pressure
  3. customthe residue was partitioned between water and ethyl acetate (200 mL each)
  4. extractionThe aqueous layer was extracted with ethyl acetate (3×200 mL)
  5. washthe combined organic layers were then washed with water and brine (200 mL each)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-7fc712df9bea40238aa90ddb61a7176d
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094896B2

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