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1-Iodopropane → 1-[3-(Methyloxy)-4-nitrophenyl]-4-propylpiperazine

HRID 419545
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HRID 419545 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10].I[CH2:19][CH2:20][CH3:21].C([O-])(O)=O.[Na+]>C(#N)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:12]2[CH2:17][CH2:16][N:15]([CH2:19][CH2:20][CH3:21])[CH2:14][CH2:13]2)[CH:6]=[CH:7][C:8]=1[N+:9]([O-:11])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 336431-IodopropaneHCID 516892Sodium BicarbonateHCID 39674091-(3-Methoxy-4-nitrophenyl)piperazine

생성물 1

HCID 598602661-[3-(Methyloxy)-4-nitrophenyl]-4-propylpiperazine수율 35.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-[3-(methyloxy)-4-nitrophenyl]piperazine (Example 135, step A) (0.50 g, 2.1 mmol) and 1-iodopropane (0.72 g, 4.22 mmol) was stirred in acetonitrile (42 mL) at rt under N2. To this mixture was added NaHCO3 (0.27 g, 2.5 mmol). The reaction was then heated to reflux and stirred for 24 h. The reaction was cooled to rt, concentrated under vacuum and the residue chromatographed on silica gel to give the title compound of step A (206 mg, 0.74 mmol, 35%) as a yellow oil. MS (ESI): 280 [M+H]+.

후처리

  1. temperatureThe reaction was then heated
  2. temperatureto reflux
  3. concentrationconcentrated under vacuum
  4. customthe residue chromatographed on silica gel

출처 및 근거

ORD 기록
ord-48c86d5449d84da390555cdf20b33c31
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093239B2

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