Reaction #2460318

ord-1ccfa20b304041a5a551b2cc18a61144

Reaction equation

[F][Sb-]([F])([F])([F])([F])[F].[Na+]
sodium hexafluoroantimonate
CCCCc1ccc(N(c2ccc(/C=C/c3ccc(N(c4ccc(CCCC)cc4)c4cccc([SH+]CCc5ccccc5)c4)cc3)cc2)c2cccc([SH+]CCc3ccccc3)c2)cc1.O=S(=O)([O-])C(F)(F)F.O=S(=O)([O-])C(F)(F)F
trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl)methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium triflate
CCCCc1ccc(N(c2ccc(/C=C/c3ccc(N(c4ccc(CCCC)cc4)c4cccc([SH+]CCc5ccccc5)c4)cc3)cc2)c2cccc([SH+]CCc3ccccc3)c2)cc1.O=S(=O)([O-])C(F)(F)F.O=S(=O)([O-])C(F)(F)F
trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl) methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium triflate
CCCCc1ccc(N(c2ccc(/C=C/c3ccc(N(c4ccc(CCCC)cc4)c4cccc([SH+]CCc5ccccc5)c4)cc3)cc2)c2cccc([SH+]CCc3ccccc3)c2)cc1.[F][Sb-]([F])([F])([F])([F])[F].[F][Sb-]([F])([F])([F])([F])[F]
trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl)methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium hexafluoroantimonate
Yield 83.2%

Conditions

Temperature
0°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherthe yellow oil that formed
  2. 2
    FiltrationThe yellow solid was collected by filtration
  3. 3
    Washwashed four times with water and three times with ether
  4. 4
    OtherNMR-pure product was obtained without further purification in 83.2% yield (0.85 g)

Procedure

trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl)methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium triflate (20) (0.85 g 0.81 mmol) was dissolved in acetone (10 ml). To this solution was added 10 ml of an aqueous solution of sodium hexafluoroantimonate (0.84 g, 3.25 mmol). The resultant mixture was stirred two days with slow evaporation of acetone in the dark at room temperature. The mixture was allowed to cool at 0° C., the yellow oil that formed solidified. The yellow solid was collected by filtration and washed four times with water and three times with ether. NMR-pure product was obtained without further purification in 83.2% yield (0.85 g). 1H NMR (CD3COCD3, 500 MHz) δ ppm: 6.9-7.7 (m, 36H, 34 Ar—H, 2 ═CH), 5.27 (d, 2J=12.5 Hz, 2H, SCH2), 5.02 (d, 2J=12.5 Hz, 2H, SCH2), 3.52 (s, 6H, CH3), 2.63 (t, J=7.7 Hz, CH2, 4H), 1.61 (m, CH2, 4H), 1.36 (m, CH2, 4H), 0.95 (t, J=7.2 Hz, CH3, 6H)13 C NMR (CD3COCD3, 125.7 MHz) δppm: 149.3, 145.6, 143.5, 139.9, 133.5, 131.9, 130.7, 130.0, 129.8, 129.3, 127.9, 127.7, 127.1, 126.5, 125.6, 124.5, 123.8, 123.4, 121.7, 51.0, 34.7, 33.5, 24.5, 22.1, 13.3.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07459106B2uspto-grants-2008_12