تفاعل #2161239

ord-e10bcd3a857e41448b4796a72dc2cde4

معادلة التفاعل

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

المذيبات

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىprepared in Synthesis Example 14
  2. 2
    درجة الحرارةwas heated
  3. 3
    غسيلThe organic layer was washed with 30 g of water three times
  4. 4
    تركيزconcentrated
  5. 5
    workup.ADDITIONDiethyl ether was added to the
  6. 6
    تركيزconcentrate for crystallization
  7. 7
    ترشيحThe crystals were filtered
  8. 8
    أخرىdried
  9. 9
    أخرىobtaining the target compound in an amount of 4.9 g

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07919226B2uspto-grants-2011_04