2-Aminocyclohex-1-ene-1-carbonitrile → 2-aminocyclohexane-1-carbonitrile
反応式
[NH2:1][C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]=1[C:8]#[N:9].[BH3-]C#N.[Na+]>CO.C(O)(=O)C.C(OCC)(=O)C>[NH2:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[C:8]#[N:9]参加物
6
実験手順
To a cold solution of 2-aminocyclohex-1-enecarbonitrile (I-7a: 50 mg, 0.41 mmol) in methanol (3 mL) was added NaCNBH3 (103 mg, 1.64 mmol) and acetic acid (5 drops) at 0° C. The resulting mixture was stirred at room temperature for 16h. The reaction mixture was diluted with ethyl acetate and the organic layer was washed with saturated NaHCO3, brine, dried over anhydrous Na2SO4 and concentrated to afford 40 mg (78%) of diastereomeric mixture of 2-aminocyclohexanecarbonitrile (I-7b) as a gum.
後処理
- washthe organic layer was washed with saturated NaHCO3, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-362529fe20684a55b771015a2944a1df
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447039B2
反応ノート
読み込み中…