Реакция #2161239

ord-e10bcd3a857e41448b4796a72dc2cde4

Уравнение реакции

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

Растворители

Условия реакции

Температура
40°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеprepared in Synthesis Example 14
  2. 2
    Температураwas heated
  3. 3
    ПромывкаThe organic layer was washed with 30 g of water three times
  4. 4
    Концентрированиеconcentrated
  5. 5
    workup.ADDITIONDiethyl ether was added to the
  6. 6
    Концентрированиеconcentrate for crystallization
  7. 7
    ФильтрацияThe crystals were filtered
  8. 8
    Другоеdried
  9. 9
    Другоеobtaining the target compound in an amount of 4.9 g

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07919226B2uspto-grants-2011_04