Hydrazine hydrate (1:1) → 3,3-dimethylbutanohydrazide
반응식
[CH3:1][C:2]([CH3:9])([CH3:8])[CH2:3][C:4](OC)=[O:5].O.[NH2:11][NH2:12]>CCO>[CH3:1][C:2]([CH3:9])([CH3:8])[CH2:3][C:4]([NH:11][NH2:12])=[O:5]참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
To a mixture of methyl 3,3-dimethylbutanoate (500 mg, 3.84 mmol) in EtOH (12 ml) was added hydrazine monohydrate (1.87 ml, 38.4 mmol). The mixture was heated to 80° C. under reflux for overnight. The reaction was cooled back down to room temperature and concentrated to dryness affording a crude residue. The residue was dried under high vacuum to afford the title compound as crystalline solid (90 mg, 18% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.69-9.12 (s, 1H) 4.13 (br. s, 2H) 1.89 (s, 2H) 0.94 (s, 9H).
후처리
- temperatureunder reflux for overnight
- temperatureThe reaction was cooled back down to room temperature
- concentrationconcentrated to dryness
- customaffording a crude residue
- customThe residue was dried under high vacuum
출처 및 근거
- ORD 기록
- ord-60863055d78c4c3d87c719c0ef7c7e81
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08993619B2
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