p-Fluoronitrobenzene → 1-Methyl-4-(4-nitrophenyl)piperazine

HRID 271127노트

반응식

HRID 271127 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>CS(C)=O>[CH3:11][N:12]1[CH2:17][CH2:16][N:15]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=2)[CH2:14][CH2:13]1

참가 물질

4

반응물 2

HCID 9590p-FluoronitrobenzeneHCID 531671-Methylpiperazine

생성물 1

HCID 28251981-Methyl-4-(4-nitrophenyl)piperazine

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 1-fluoro-4-nitrobenzene (2.54 mL, 24 mmol) and N-methylpiperazine (2.22 mL, 20 mmol) was dissolved in DMSO (25 mL) and irradiated in a microwave oven (max power 250 W, 160° C.) for 10 min, then cooled to room temperature. The solvent was removed under high vacuum, and the residue was dissolved in EtOAc and extracted with 0.5M aqueous HCl. The aqueous extracts were combined, basified to pH 8, and extracted with EtOAc. The organic layer was washed with brine, and then dried over MgSO4. Evaporation of the solvent provided the crude 1-methyl-4-(4-nitrophenyl)piperazine as an brown oil.

후처리

  1. customirradiated in a microwave oven (max power 250 W, 160° C.) for 10 min
  2. customThe solvent was removed under high vacuum
  3. dissolutionthe residue was dissolved in EtOAc
  4. extractionextracted with 0.5M aqueous HCl
  5. extractionextracted with EtOAc
  6. washThe organic layer was washed with brine
  7. dry with materialdried over MgSO4
  8. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-f7f4af4ecf7d49978c36d2a04c4d7401
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452887B2

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