Reacción #2195488

ord-fd466009186449ee86a027ef269d8b74

Ecuación de reacción

Cl
hydrochloric acid
CCN(CC)CC
Triethylamine
CC(C)(C)C(=O)OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-].[Na+]
sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate
ClCCl
dichloromethane
CC(C)(C)C(=O)OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-].C[NH+](C)C
trimethylammonium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate
Rendimiento 75.0%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwere added, whereupon the mixture
  2. 2
    OtroThe organic layer was separated
  3. 3
    Lavadowashed with water
  4. 4
    LavadoFrom the organic layer as washed
  5. 5
    workup.DISTILLATIONthe dichloromethane was distilled off in vacuum
  6. 6
    workup.ADDITIONDiethyl ether was added to the residue for recrystallization
  7. 7
    FiltraciónThe crystals were filtered
  8. 8
    Otrodried
  9. 9
    Otroobtaining the target compound in a yield of 75%

Procedimiento

Triethylamine was dissolved in cold water. To the solution, hydrochloric acid was added, and sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate prepared in Synthesis Example 27 and dichloromethane were added, whereupon the mixture was stirred. The organic layer was separated and washed with water. From the organic layer as washed, the dichloromethane was distilled off in vacuum. Diethyl ether was added to the residue for recrystallization. The crystals were filtered and dried, obtaining the target compound in a yield of 75%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07514202B2uspto-grants-2009_04