Hydroxyamine hydrochloride → 4-Ethoxy-benzofuran-3-one oxime
反応式
[CH2:1]([O:3][C:4]1[C:9]2[C:10](=O)[CH2:11][O:12][C:8]=2[CH:7]=[CH:6][CH:5]=1)[CH3:2].C([O-])(=O)C.[Na+].Cl.[NH2:20][OH:21]>C(O)C.O>[CH2:1]([O:3][C:4]1[C:9]2[C:10](=[N:20][OH:21])[CH2:11][O:12][C:8]=2[CH:7]=[CH:6][CH:5]=1)[CH3:2]参加物
6
反応条件
- 温度
- 23 °C
実験手順
A mixture of 4-ethoxy-benzofuran-3-one (CAS no: 7169-36-0) (4.18 g, 23.5 mmol), sodium acetate (3.96 g, 48.3 mmol) and hydroxylamine hydrochloride (3.34 g, 48.1 mmol) in ethanol (30 mL) was refluxed for 16 h. Cooled to 23° C., diluted with water (50 mL), filtered the precipitate off, washed with water, ethanol and diethyl ether and dried in high vacuum to give the title compound as a white solid (4.2 g, 93%); MS: m/e=194.3 (M+H+).
後処理
- temperaturewas refluxed for 16 h
- filtrationfiltered the precipitate off,
- washwashed with water, ethanol and diethyl ether
- customdried in high vacuum
出典と根拠
- ORDレコード
- ord-f20a39b79b404aa2a5afa4ebd3b9998c
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183380B2
反応ノート
読み込み中…