反応 #2161239

ord-e10bcd3a857e41448b4796a72dc2cde4

反応方程式

CC(C)(C)Oc1ccc([S+](c2ccccc2)c2ccccc2)cc1.O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1
4-tert-butoxyphenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate
CS(=O)(=O)O
Methanesulfonic acid
O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1.Oc1ccc([S+](c2ccccc2)c2ccccc2)cc1
(4-hydroxyphenyl)diphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他prepared in Synthesis Example 14
  2. 2
    温度was heated
  3. 3
    洗浄The organic layer was washed with 30 g of water three times
  4. 4
    濃縮concentrated
  5. 5
    workup.ADDITIONDiethyl ether was added to the
  6. 6
    濃縮concentrate for crystallization
  7. 7
    ろ過The crystals were filtered
  8. 8
    その他dried
  9. 9
    その他obtaining the target compound in an amount of 4.9 g

実験手順

In 60 g of dichloromethane was dissolved 6.7 g of 4-tert-butoxyphenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate (PAG4) prepared in Synthesis Example 14. Methanesulfonic acid, 0.1 g, was added to the solution, which was heated and stirred at 40° C. for 3 hours. The organic layer was washed with 30 g of water three times, and concentrated. Diethyl ether was added to the concentrate for crystallization. The crystals were filtered and dried, obtaining the target compound in an amount of 4.9 g.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07919226B2uspto-grants-2011_04