Heptanedinitrile → 2-Aminocyclohex-1-ene-1-carbonitrile
反応式
[C:1](#[N:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[N:8].CC([O-])(C)C.[K+]>O>[NH2:8][C:7]1[CH2:6][CH2:5][CH2:4][CH2:3][C:2]=1[C:1]#[N:9]参加物
4
反応条件
- 温度
- 80 °C
実験手順
A stirred mixture of 1,7-heptanedinitrile (24.44 g, 0.2 mol) and t-BuOK (22.44 g, 0.2 mol) was heated at 80° C. for 3 h under nitrogen. The mixture was then cooled down to room temperature and stored at that temperature overnight. The residue was treated with water, and extracted with ether (2×). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified by recrystallization from MeOH to give the title compound as a white solid (18.2 g, 75%). 1H NMR (400 MHz, CDCl3) δ 1.58-1.71 (m, 4H), 2.12-2.20 (m, 4H), 4.23 (bs, 2H). MS 123 (MH+).
後処理
- temperatureThe mixture was then cooled down to room temperature
- customstored at that temperature overnight
- extractionextracted with ether (2×)
- washThe combined organic layers were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by recrystallization from MeOH
出典と根拠
- ORDレコード
- ord-9d3701d78da347b4913d69e523ac2280
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08633186B2
反応ノート
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