HCID 19754698, 화합물 → HCID 19754672, 화합물
반응식
[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]1참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-c113d66ae96c4a12a9ca290cbbd3e968
- 출처 데이터셋
- uspto-grants-1993_06
- 특허 번호
- US05223526
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