Hydroxyamine hydrochloride → 5-Bromo-2,3-dihydro-1H-inden-1-one Oxime
반응식
[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]2참가 물질
4
실험 절차
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
후처리
- 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
출처 및 근거
- ORD 기록
- ord-121a97ab78944121ab84896d2a3cee3e
- 출처 데이터셋
- uspto-grants-2014_01
- 특허 번호
- US08633237B2
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