Reaction equation
[N+:1]([O-:4])([O-:3])=[O:2].[Ag+:5].[CH2:6]([S:8][CH2:9][CH3:10])[CH3:7]>C(#N)C>[N+:1]([O-:4])([O-:3])=[O:2].[Ag+:5].[CH2:6]([S:8][CH2:9][CH3:10])[CH3:7]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a 100 ml round bottom flask was sequentially added 10 mmol (1.69 g) of silver nitrate 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 ivory solid matter. 1H-NMR result in CD3CN is as follows: 1.34 (t, 7.36 Hz, 6H), 2.76(q, 7.36 Hz, 4H).
Workup
- 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 ivory solid matter
- custom1H-NMR result in CD3CN
Sources & evidence
- ORD record
- ord-bff01c618220429d988283336dd2d59e
- Source dataset
- uspto-grants-2005_11
- Patent number
- US06965045B2
Linked notes
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