Hydroxyamine hydrochloride → 5-Bromo-2,3-dihydro-1H-inden-1-one Oxime
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=O)[CH2:6][CH2:5]2.Cl.[NH2:13][OH:14]>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)/[C:7](=[N:13]/[OH:14])/[CH2:6][CH2:5]2参加物
4
実験手順
5-bromo-2,3-dihydro-1H-inden-1-one (25 g, 118 mmol) and hydroxylamine hydrochloride (12.35 g, 178 mmol) were heated in Ethanol (150 mL) for 5 hours with stirring. The solvent was evaporated in vacuo and remaining solid partitioned between H2O and EtOAc. The organic layer was separated and washed with brine (2×), dried on Na2SO4 and solvent evaporated in vacuo to afford the title compound as a light brown solid (23.6 g, 87%). MS (ESI): m/z [M+H]+ 227.0
後処理
- customThe solvent was evaporated in vacuo
- custompartitioned between H2O and EtOAc
- customThe organic layer was separated
- washwashed with brine (2×)
- customdried on Na2SO4 and solvent
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-121a97ab78944121ab84896d2a3cee3e
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08633237B2
反応ノート
読み込み中…