Реакция #2195488

ord-fd466009186449ee86a027ef269d8b74

Уравнение реакции

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
Выход 75.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwere added, whereupon the mixture
  2. 2
    ДругоеThe organic layer was separated
  3. 3
    Промывкаwashed with water
  4. 4
    ПромывкаFrom 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
    ФильтрацияThe crystals were filtered
  8. 8
    Другоеdried
  9. 9
    Другоеobtaining the target compound in a yield of 75%

Методика

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%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07514202B2uspto-grants-2009_04