Reaktion #2175463
ord-490d49d633c0425fa1afcfc8710ff1e0
Reaktionsgleichung
sodium disulfite
sodium cyanide
4-trifluoroethoxycyclohexanone
→
1-Hydroxy-4-trifluoroethoxycyclohexanecarbonitrile
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONare then added dropwise
- 2Temperaturwith cooling at 25-30° C. over a period of 30 min
- 3workup.STIRRINGthe mixture is stirred at room temperature
- 4ExtraktionThe aqueous phase is extracted 3× with in each case 90 ml of toluene
- 5Einengenconcentrated under reduced pressure
Vorschrift
13.74 g of sodium cyanide are dissolved in 200 ml of water. Over a period of 30 min, 50 g of 4-trifluoroethoxycyclohexanone are then added dropwise at 20-28° C. with slight cooling. The mixture is stirred at 25° C. for 5 minutes, and 31.48 g of sodium disulfite, dissolved in 100 ml of water, are then added dropwise with cooling at 25-30° C. over a period of 30 min. With monitoring by thin-layer chromatography, the mixture is stirred at room temperature. The aqueous phase is extracted 3× with in each case 90 ml of toluene. The organic phases are combined and concentrated under reduced pressure.