Sodium Carbonate → HCID 118162236、化合物
反応式
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=O)[C:3]1([CH3:10])[CH3:9].Cl.[NH2:12][OH:13].C(=O)([O-])[O-].[Na+].[Na+]>CCO.O>[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=[N:12][OH:13])[C:3]1([CH3:10])[CH3:9]参加物
6
反応条件
- 温度
- 25 °C
実験手順
A mixture of 3-hydroxy-2,2-dimethylcyclohexanone (1.6 g, crude), hydroxylamine hydrochloride (2.98 g, 42.9 mmol) and sodium carbonate (4.54 g, 42.9 mmol) in EtOH (30 mL) and water (3 mL) was stirred at 25° C. for 6 h. After removal of EtOH, the residue was extracted with ethyl acetate (2×200 mL). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated to afford the title compound (1.8 g, crude). MS (ESI) m/z 158.2 [M+H]+.
後処理
- customAfter removal of EtOH
- extractionthe residue was extracted with ethyl acetate (2×200 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9d39f206ef18475a96d147d6ca4602ab
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09156798B2
反応ノート
読み込み中…