반응 #2161239

ord-e10bcd3a857e41448b4796a72dc2cde4

반응 방정식

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

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared in Synthesis Example 14
  2. 2
    온도was heated
  3. 3
    세척The organic layer was washed with 30 g of water three times
  4. 4
    농축concentrated
  5. 5
    workup.ADDITIONDiethyl ether was added to the
  6. 6
    농축concentrate for crystallization
  7. 7
    여과The crystals were filtered
  8. 8
    기타dried
  9. 9
    기타obtaining the target compound in an amount of 4.9 g

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07919226B2uspto-grants-2011_04