Hydroxyamine hydrochloride → 2-Amino-pyridine-3-carbaldehyde oxime
反応式
[NH2:1][C:2]1[C:7]([CH:8]=O)=[CH:6][CH:5]=[CH:4][N:3]=1.Cl.[NH2:11][OH:12]>N1C=CC=CC=1>[NH2:1][C:2]1[C:7]([CH:8]=[N:11][OH:12])=[CH:6][CH:5]=[CH:4][N:3]=1参加物
4
実験手順
To a solution of 2-amino-3-formylpyridine (1.00 g, 8.19 mmol) in pyridine (20 mL) was added hydroxylamine hydrochloride (854 mg, 12.3 mmol) at room temperature, which was stirred for 1 hour and 40 minutes at room temperature. The reaction solution was partitioned into water and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=10:1) to obtain the title compound (951 mg, 85%).
後処理
- customThe reaction solution was partitioned into water and ethyl acetate
- washThe organic layer was washed with water and saturated aqueous sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated under a reduced pressure
- customThe residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=10:1)
出典と根拠
- ORDレコード
- ord-baa4fbef9e2643f6b1ead7f2fa670978
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08158657B2
反応ノート
読み込み中…