Hydrazine → 2,4-Dimethoxybenzohydrazide
반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:5]=1[O:12][CH3:13].[NH2:15][NH2:16]>CO>[CH3:13][O:12][C:5]1[CH:6]=[C:7]([O:10][CH3:11])[CH:8]=[CH:9][C:4]=1[C:3]([NH:15][NH2:16])=[O:2]참가 물질
4
실험 절차
Ex-109A: A solution of 2,4-dimethoxy-benzoic acid methyl ester (4.24 g, 21.6 mmol) and hydrazine (3.4 mL, 108.1 mmol) in methanol (50 mL) was refluxed overnight. Solvent was removed under reduced pressure. The residue was re-dissolved in ethyl acetate. The solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine, dried over sodium carbonate and concentrated to afford 2,4-dimethoxy-benzoic acid hydrazide (3.31 g, 78%) as a white solid: 1H NMR (CDCl3) δ 8.77 (bs, 1H), 8.15 (d, J=8.8 Hz, 1H), 6.58 (dd, J=8.8, 2.2 Hz, 1H), 6.46 (d, J=2.2 Hz, 1H), 4.10 (bs, 2H), 3.91 (s, 3H), 3.83 (s, 3H).
후처리
- customSolvent was removed under reduced pressure
- dissolutionThe residue was re-dissolved in ethyl acetate
- washThe solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine
- dry with materialdried over sodium carbonate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-665a71c8df494a06987f1f3e49f3c7d1
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07094801B2
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