Reacción #340082

ord-9c58d534780a4f299c49d84e8b761102

Ecuación de reacción

Cl
hydrochloric acid
CCN(CC)CC
Triethylamine
O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1.[Na+]
sodium 1,1,3,3,3-pentafluoro-2-(benzoyloxy)propanesulfonate
ClCCl
dichloromethane
CC[NH+](CC)CC.O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1
desired product
Rendimiento 75.0%
CC[NH+](CC)CC.O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1
triethylammonium 1,1,3,3,3-pentafluoro-2-(benzoyloxy)propanesulfonate
Rendimiento 75.0%

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe pH of the reaction liquid
  2. 2
    LavadoThe separated organic layer was washed with water, and dichloromethane
  3. 3
    Otrowas removed under reduced pressure from the washed organic layer
  4. 4
    OtroTo the residue thus obtained
  5. 5
    FiltraciónThe resultant was filtrated
  6. 6
    Otrodried

Procedimiento

Triethylamine was dissolved in cold water, and hydrochloric acid was added thereto to adjust the pH of the reaction liquid to fall within a range of 1 to 3. Then sodium 1,1,3,3,3-pentafluoro-2-(benzoyloxy)propanesulfonate and dichloromethane were added thereto and stirred. The separated organic layer was washed with water, and dichloromethane was removed under reduced pressure from the washed organic layer. To the residue thus obtained, diethyl ether was added for recrystallization. The resultant was filtrated and dried to obtain a desired product at a yield of 75%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07871761B2uspto-grants-2011_01