反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[O:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][C:16]#[N:17])[CH2:9][CH2:8]1>C1COCC1.O>[O:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH2:9][CH2:8]1参加物
5
反応条件
- 温度
- 0 °C
実験手順
To anhydrous THF (70 mL) was added LiAlH4 (5.37 g, 142 mmol) in one portion. The mixture was stirred at 0° C. for 20 min, and a solution of 4-morpholinobutanenitrile (7.26 g, 47 mmol) in anhydrous THF (40 mL) was added dropwise. Upon the end of addition the mixture was refluxed for 4 h, then cooled to 0° C., diluted with water (20 mL) and filtered. The filtrate was concentrated in vacuo to give the crude product for the next step without further purification.
後処理
- additionUpon the end of addition the mixture
- temperaturewas refluxed for 4 h
- temperaturecooled to 0° C.
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-2c9a79470dd24e1c8cfc412f9d1e7bf0
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434695B2
関連ノート
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