Réaction #2175463

ord-490d49d633c0425fa1afcfc8710ff1e0

Équation de réaction

O=S([O-])OS(=O)[O-].[Na+].[Na+]
sodium disulfite
[C-]#N.[Na+]
sodium cyanide
O=C1CCC(OCC(F)(F)F)CC1
4-trifluoroethoxycyclohexanone
N#CC1(O)CCC(OCC(F)(F)F)CC1
1-Hydroxy-4-trifluoroethoxycyclohexanecarbonitrile

Solvants

Conditions de réaction

Température
25°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONare then added dropwise
  2. 2
    Températurewith cooling at 25-30° C. over a period of 30 min
  3. 3
    workup.STIRRINGthe mixture is stirred at room temperature
  4. 4
    ExtractionThe aqueous phase is extracted 3× with in each case 90 ml of toluene
  5. 5
    Concentrationconcentrated under reduced pressure

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08435549B2uspto-grants-2013_05