Hydrazine hydrate (1:1) → 6-Methyl-5-propyl-4,5-dihydropyridazin-3(2H)-one
反応式
[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]=1参加物
4
反応条件
- 温度
- 85 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-d7a20aba0c274203b2a8b46e4290b807
- 出典データセット
- uspto-grants-2006_10
- 特許番号
- US07122546B2
反応ノート
読み込み中…