Water → 1-Azabicyclo[4.3.1]decane-8-carbonitrile
反応式
[H-].[Na+].CC(C)([O-])C.[K+].Cl[CH2:10][CH:11]1[CH2:17][CH2:16][CH2:15][CH2:14][N:13]([CH2:18][CH2:19][C:20]#[N:21])[CH2:12]1.O>CN(C=O)C>[C:20]([CH:19]1[CH2:18][N:13]2[CH2:12][CH:11]([CH2:17][CH2:16][CH2:15][CH2:14]2)[CH2:10]1)#[N:21]参加物
6
反応条件
- 温度
- 70 °C
実験手順
To a stirred suspension of sodium hydride (1.5 g, 80%) and potassium t-butoxide (0.5 g) in DMF (100 ml) was added 3-chloromethyl-1-(2'-cyanoethyl)homopiperidine (D6) (5 g) and the reaction mixture was carefully warmed to 70° C. for 1 hour. On cooling, water (5 ml) was carefully added and the DMF was removed by rotary evaporation. Extraction of the residue with ethyl acetate, concentration and distillation afforded the (±) 8-cyano-1-azabicyclo-[4,3,1]-decane (D7) (4.0 g, 90%) bp 68°-73°/0.1 mm.
後処理
- temperatureOn cooling
- customthe DMF was removed by rotary evaporation
- extractionExtraction of the residue
- concentrationwith ethyl acetate, concentration and distillation
出典と根拠
- ORDレコード
- ord-d160eeabd4bc4c15adc4c31da5ec7c63
- 出典データセット
- uspto-grants-1989_08
- 特許番号
- US04857647
反応ノート
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