Hydrazine hydrate (1:1) → 6-Methyl-5-propyl-4,5-dihydropyridazin-3(2H)-one
반응식
[NH2:1][NH2:2].O.[C:4]([CH:7]([CH2:12][CH2:13][CH3:14])[CH2:8][C:9](O)=[O:10])(=O)[CH3:5]>CCO>[CH3:5][C:4]1[CH:7]([CH2:12][CH2:13][CH3:14])[CH2:8][C:9](=[O:10])[NH:1][N:2]=1참가 물질
4
반응 조건
- 온도
- 85 °C
실험 절차
NH2NH2—H2O (6.94 ml, 143 mmol) is added to a solution of 3-acetyl-hexanoic acid (18.8 g, 119 mmol) in EtOH (150 ml), and the mixture is refluxed (oil bath 85° C.) for 4 hours. The solvent is removed in vacuo and water (100 ml) and EtOAc (100 ml) are added to the residue. The layers are separated and the aqueous layer is extracted with EtOAc (3×100ml). The combined extracts are washed with brine (150 ml), dried (Na2SO4) and evaporated. 6-methyl-5propyl-4,5-dihydropyridazin-3-one is obtained as a light yellow oil, and is used in the next step.
후처리
- customThe solvent is removed in vacuo and water (100 ml) and EtOAc (100 ml)
- additionare added to the residue
- customThe layers are separated
- extractionthe aqueous layer is extracted with EtOAc (3×100ml)
- washThe combined extracts are washed with brine (150 ml)
- dry with materialdried (Na2SO4)
- customevaporated
출처 및 근거
- ORD 기록
- ord-d7a20aba0c274203b2a8b46e4290b807
- 출처 데이터셋
- uspto-grants-2006_10
- 특허 번호
- US07122546B2
반응 노트
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