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

HRID 469833
ノート
印刷プレビュー

反応式

HRID 469833 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-365271319e324cc3a360d9131a2f9097
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629168B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート