반응 #578431

ord-497033c00cf94772b16745e935eee3ec

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타synthesized in Synthesis Example 9
  2. 2
    기타The organic layer was separated
  3. 3
    세척washed with 20 g of water three times
  4. 4
    농축The organic layer was concentrated
  5. 5
    workup.ADDITION10 g of diisopropyl ether was added to the residue for crystallization
  6. 6
    여과The crystals were filtered
  7. 7
    기타dried
  8. 8
    기타obtaining the target compound

실험 절차

To 62 g of dichloromethane were added an amount (corresponding to 0.031 mole) of the triphenylsulfonium chloride aqueous solution of Synthesis Example 1 and 1.1 g (0.033 mole) of sodium 1,1-difluoro-2-tosyloxyethanesulfonate synthesized in Synthesis Example 9, followed by stirring. The organic layer was separated and washed with 20 g of water three times. The organic layer was concentrated and 10 g of diisopropyl ether was added to the residue for crystallization. The crystals were filtered and dried, obtaining the target compound. White crystals, 1.3 g (yield 74%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07531290B2uspto-grants-2009_05