Bromine → 6-Methyl-5-propylpyridazin-3(2H)-one
反応式
[CH3:1][C:2]1[CH:3]([CH2:9][CH2:10][CH3:11])[CH2:4][C:5](=[O:8])[NH:6][N:7]=1.BrBr>CC(O)=O>[CH3:1][C:2]1[C:3]([CH2:9][CH2:10][CH3:11])=[CH:4][C:5](=[O:8])[NH:6][N:7]=1参加物
4
反応条件
- 温度
- 85 °C
実験手順
To a solution of 6-methyl-5-propyl-4,5-dihydropyridazin-3-one (16.7 g, 108 mmol) in HOAc (200 ml) heated to 85° C., is added Br2 (5.5 ml, 108 mmol) dropwise. After the addition, the mixture is stirred at 85° C. for 1 hour. The solvent is removed in vacuo and the residue is dissolved in EtOAc (250 ml) and washed with NaHCO3 (200 ml) followed by Na2S2O3 saturated solution (50 ml) and brine (200 ml). The organic phase is dried (Na2SO4) and evaporated. The resulting yellow solid is used in next step without further purification.
後処理
- additionAfter the addition
- customThe solvent is removed in vacuo
- dissolutionthe residue is dissolved in EtOAc (250 ml)
- washwashed with NaHCO3 (200 ml)
- dry with materialThe organic phase is dried (Na2SO4)
- customevaporated
- customThe resulting yellow solid is used in next step without further purification
出典と根拠
- ORDレコード
- ord-be1966c2107a4fd2afe5505c9a173e62
- 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…