Reaktion #1062012

Reaktionsgleichung

4,4,5-trimethyl-8-chlorothiochroman-6-carboxylic acid-1,1-dioxide

→

4,4,5-trimethylthiochroman-6-carboxylic acid-1,1-dioxide

Ausbeute 78.0%

Lösungsmittel

ethanol

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Temperaturthe mixture was refluxed
3. 3
   Temperaturunder heat for 5 hours
4. 4
   workup.ADDITIONwas added
5. 5
   Sonstigethe zinc powder was removed by filtration
6. 6
   Extraktionthe remainder was extracted with ethyl acetate
7. 7
   WaschenThe extract was washed with a saturated sodium chloride aqueous solution
8. 8
   Trocknendried over anhydrous sodium sulfate
9. 9
   workup.DISTILLATIONThe ethyl acetate was distilled off under reduced pressure

Vorschrift

0.88 Gram (2.90 mmol) of 4,4,5-trimethyl-8-chlorothiochroman-6-carboxylic acid-1,1-dioxide was dissolved in ethanol having a water content of 60%, 0.55 g (8.70 mmol) of a zinc powder was added, and the mixture was refluxed under heat for 5 hours. After the completion of the reaction, 50 ml of water was added, the zinc powder was removed by filtration, and the remainder was extracted with ethyl acetate. The extract was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The ethyl acetate was distilled off under reduced pressure to give 0.60 g (yield 78%) of 4,4,5-trimethylthiochroman-6-carboxylic acid-1,1-dioxide.

Quelle