反応式
[N:1]1([CH2:8][CH2:9][NH2:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(#N)CO>O>[CH2:5]1[CH2:6][CH2:7][N:1]([CH2:8][C:9]#[N:10])[CH2:2][CH2:3][CH2:4]1参加物
4
反応条件
- 温度
- 70 °C
実験手順
Azepane (289) (4.9 mL, 43.8 mmol) was added dropwise to a stirred aqueous solution of glycolonitrile (55%, 5.0 g, 48.2 mmol) at 5° C. and the solution was stirred at 70° C. for 30 min. The solution was cooled, diluted with water (20 mL), washed with Et2O (3×50 mL). The organic fraction was dried and the solvent evaporated to give nitrile 290 (5.58 g, 92%) as a colourless oil: 1H NMR δ 3.56 (s, 2H, CH2CN), 2.71 (br dd, J=5.8, 5.5 Hz, 4H, 2×CH2N), 1.67-1.73 (m, 4H, 2×CH2), 1.59-1.64 (m, 4H, 2×CH2).
後処理
- temperatureThe solution was cooled
- washwashed with Et2O (3×50 mL)
- customThe organic fraction was dried
- customthe solvent evaporated
出典と根拠
- ORDレコード
- ord-852a5c1da3494ff4b3dbe92e14b41e55
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07989451B2
関連ノート
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