反応 #312587

ord-f9eabe6b564c4287b4b398c47b0987fc

反応方程式

[Cl-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium chloride
O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1.[Na+]
sodium 2-benzoyloxy-1,1,3,3,3-pentafluoro-propane-1-sulfonate
O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1.c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium 2-benzoyloxy-1,1,3,3,3-pentafluoropropane-1-sulfonate
収率 75.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他synthesized in Synthesis Example 9
  2. 2
    その他The organic layer was separated
  3. 3
    洗浄washed with 50 g of water three times
  4. 4
    濃縮The organic layer was concentrated
  5. 5
    workup.ADDITION25 g of diethyl ether was added to the residue for crystallization
  6. 6
    ろ過The crystals were filtered
  7. 7
    その他dried
  8. 8
    その他obtaining the target compound

実験手順

To 50 g of dichloromethane were added an amount (corresponding to 0.011 mole) of the triphenylsulfonium chloride aqueous solution of Synthesis Example 1 and 3.6 g (0.01 mole) of sodium 2-benzoyloxy-1,1,3,3,3-pentafluoro-propane-1-sulfonate synthesized in Synthesis Example 9, followed by stirring. The organic layer was separated and washed with 50 g of water three times. The organic layer was concentrated and 25 g of diethyl ether was added to the residue for crystallization. The crystals were filtered and dried, obtaining the target compound. White crystals, 4.5 g (yield 75%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07556909B2uspto-grants-2009_07