Hydrazine hydrate (1:1) → 6-Methyl-5-propyl-4,5-dihydropyridazin-3(2H)-one
反応式
[C:1]([CH:4]([CH2:9][CH2:10][CH3:11])[CH2:5][C:6](O)=[O:7])(=O)[CH3:2].[NH2:12][NH2:13].O>CCO>[CH3:2][C:1]1[CH:4]([CH2:9][CH2:10][CH3:11])[CH2:5][C:6](=[O:7])[NH:12][N:13]=1参加物
4
反応条件
- 温度
- 85 °C
実験手順
To a solution of 3-acetyl-hexanoic acid (18.8 g, 119 mmol) in EtOH (150 ml) is added NH2NH2—H2O (6.94 ml, 143 mmol) and the mixture is refluxed (oil bath 85° C.) for 4 hours. solvent is removed in vacuo and to the residue is added water (100 ml) and EtOAc (100 ml). The layers are separated and the aqueous layer is extracted with EtOAc (3×100 ml). The combined extracts are washed with brine (150 ml), dried (Na2SO4) and evaporated. The resulting light yellow oil is used without further purification in the next step.
後処理
- customsolvent is removed in vacuo and to the residue
- additionis added water (100 ml) and EtOAc (100 ml)
- customThe layers are separated
- extractionthe aqueous layer is extracted with EtOAc (3×100 ml)
- washThe combined extracts are washed with brine (150 ml)
- dry with materialdried (Na2SO4)
- customevaporated
- customThe resulting light yellow oil is used without further purification in the next step
出典と根拠
- ORDレコード
- ord-ce27e07a9de14c9ab75b7d8850c93313
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07351826B2
反応ノート
読み込み中…