HCID 19754698、化合物 → HCID 19754672、化合物
反応式
[C:1]1(=[CH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N+:14]([O-])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>C(O)(=O)C.[Fe]>[C:1]1(=[CH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH2:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1参加物
4
実験手順
To 1-(cyclohexylidenemethyl)-2-nitrobenzene (1.6 g) in glacial acetic acid (50 mL), at 85° C., was added iron powder (2.07 g). The mixture was refluxed for 15 min. The mixture was cooled and filtered through clay. The filtrate was partitioned between EtOAc and ice water. The ethyl acetate layer was washed well with a saturated NaHCO3 solution, dried (MgSO4), and concentrated in vacuo. The residue was chromatographed on silica gel eluting with hexanes to give 2-(cyclohexylidenemethyl)aniline.
後処理
- temperatureThe mixture was refluxed for 15 min
- temperatureThe mixture was cooled
- filtrationfiltered through clay
- customThe filtrate was partitioned between EtOAc and ice water
- washThe ethyl acetate layer was washed well with a saturated NaHCO3 solution
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was chromatographed on silica gel eluting with hexanes
出典と根拠
- ORDレコード
- ord-c113d66ae96c4a12a9ca290cbbd3e968
- 出典データセット
- uspto-grants-1993_06
- 特許番号
- US05223526
反応ノート
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