反応式
[N:1]([O-:3])=[O:2].[Ag+:4].[CH2:5]([S:7][CH2:8][CH3:9])[CH3:6]>C(#N)C>[N:1]([O-:3])=[O:2].[Ag+:4].[CH2:5]([S:7][CH2:8][CH3:9])[CH3:6]参加物
4
実験手順
To a 100 ml round bottom flask was sequentially added 10 mmol (1.54 g) of silver nitrite (AgNO2) and 20 ml of acetonitrile, followed by stirring at room temperature for 5 minutes. Next, 10 mmol (0.90 g, 1.08 ml) of diethylthioether was dropwise added to the flask by means of a syringe over 10 seconds and stirred at room temperature. After stirring for 30 minutes, the reaction mixture was warmed to 50° C. and further stirred for 30 minutes. Following cooling to room temperature, the reaction mixture was filtered through a microfilter and evaporated under vacuum to produce a pale yellow solid matter. 1H-NMR result in CD3CN is as follows: 1.31 (t, 7.34 Hz, 6H), 2.72 (broad q, 7.35 Hz, 4H).
後処理
- customTo a 100 ml round bottom flask was sequentially added
- stirringstirred at room temperature
- stirringAfter stirring for 30 minutes
- temperaturethe reaction mixture was warmed to 50° C.
- stirringfurther stirred for 30 minutes
- temperatureFollowing cooling to room temperature
- filtrationthe reaction mixture was filtered through a microfilter
- customevaporated under vacuum
- customto produce a pale yellow solid matter
- custom1H-NMR result in CD3CN
出典と根拠
- ORDレコード
- ord-d50baf787a69429cbf16a064b73294cd
- 出典データセット
- uspto-grants-2005_11
- 特許番号
- US06965045B2
関連ノート
読み込み中…