Hydroxyamine hydrochloride → 2-(5-Aminoisoxazol-3-yl)-2-methylpropanenitrile
反応式
[NH2:1][C:2]([C:6]([CH3:10])([CH3:9])[C:7]#[N:8])=[CH:3][C:4]#[N:5].N[OH:12].Cl>CO>[NH2:5][C:4]1[O:12][N:1]=[C:2]([C:6]([CH3:10])([CH3:9])[C:7]#[N:8])[CH:3]=1参加物
4
反応条件
- 温度
- 40 °C
実験手順
To 3-Amino-4,4-dimethyl-pent-2-endinitrile (10.0 g, 74 mmol) in MeOH (150 mL) is added NH2OH.HCl (10.0 g, 144 mmol). The mixture is stirred at 40° C. for 7 h, concentrated, suspended in isopropyl acetate (100 mL) and washed with 4 N aq. NaOH (2×100 mL) and brine (50 mL). The extracted org. layer is concentrated to provide 7.40 g of 2-(5-Amino-isoxazol-3-yl)-2-methyl-propionitrile. Yield: 66%; ESI-MS: 152 [M+H]+; 1H-NMR (DMSO-d6): 1.6, 5.1, 6.8 ppm.
後処理
- concentrationconcentrated
- washwashed with 4 N aq. NaOH (2×100 mL) and brine (50 mL)
- concentrationlayer is concentrated
出典と根拠
- ORDレコード
- ord-517464bbbc3547638e27e1d2fb2d05a7
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08865744B1
反応ノート
読み込み中…