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Benzene, 1-fluoro-2-methyl-4-nitro- → 1-(2-Methoxy-ethyl)-4-(2-methyl-4-nitro-phenyl)-piperazine

HRID 469833
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HRID 469833 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].[CH3:12][O:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>CC(N(C)C)=O>[CH3:12][O:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][N:19]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=2[CH3:11])[CH2:18][CH2:17]1
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참가 물질

4

반응물 2

HCID 68001Benzene, 1-fluoro-2-methyl-4-nitro-HCID 27346381-(2-Methoxyethyl)piperazine

생성물 1

HCID 674588251-(2-Methoxy-ethyl)-4-(2-methyl-4-nitro-phenyl)-piperazine

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A solution of 0.95 g (6.06 mmol) 2-fluoro-5-nitrotoluene and 0.99 g (6.67 mmol) 1-(2-methoxyethyl)piperazine in 10 ml dimethylacetamide is stirred at 120° C. for 20 h. After that the reaction mixture is poured on water and extracted 3× with EtOAc. The combined organic layers are washed with water and saturated NaCl solution, dried over MgSO4, filtered and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, EtOAc) to afford the title compound as an oil.

후처리

  1. additionAfter that the reaction mixture is poured on water
  2. extractionextracted 3× with EtOAc
  3. washThe combined organic layers are washed with water and saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationthe filtrate is concentrated in vacuo
  7. customThe residue is purified by chromatography (silicagel, EtOAc)

출처 및 근거

ORD 기록
ord-365271319e324cc3a360d9131a2f9097
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629168B2

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