Tetrahydrothiophene → HCID 22280840, compound

HRID 1063502Notes

Reaction equation

HRID 1063502 reaction equation
[N+:1]([O-:4])([O-:3])=[O:2].[Ag+:5].[S:6]1[CH2:10][CH2:9][CH2:8][CH2:7]1>C(#N)C>[N+:1]([O-:4])([O-:3])=[O:2].[Ag+:5].[S:6]1[CH2:10][CH2:9][CH2:8][CH2:7]1

Participants

4

Procedure

To a 100 ml round bottom flask was sequentially added 10 mmol (1.69 g) of silver nitrate (AgNO3) and 20 ml of acetonitrile (CH3CN), followed by stirring at room temperature for 5 minutes. Next, 10 mmol (0.88 g, 0.88 ml) of tetrahydrothiophene 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 white solid matter. 1H-NMR result in CD3CN is as follows: 2.01 (m, 4H), 2.98(m, 4H).

Workup

  1. customTo a 100 ml round bottom flask was sequentially added
  2. stirringstirred at room temperature
  3. stirringAfter stirring for 30 minutes
  4. temperaturethe reaction mixture was warmed to 50° C.
  5. stirringfurther stirred for 30 minutes
  6. temperatureFollowing cooling to room temperature
  7. filtrationthe reaction mixture was filtered through a microfilter
  8. customevaporated under vacuum
  9. customto produce a white solid matter
  10. custom1H-NMR result in CD3CN

Sources & evidence

ORD record
ord-fc76136311e840c48d02f6734dc3e990
Source dataset
uspto-grants-2005_11
Patent number
US06965045B2

Reaction notes

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