反应 #2460316

ord-08a9acc61bcd4271ab7ea3f6da6f4a90

反应方程式

C[S+](C)c1cccc(N(c2ccccc2)c2ccc(C=Cc3ccc(N(c4ccccc4)c4cccc([S+](C)C)c4)cc3)cc2)c1.O=S(=O)([O-])C(F)(F)F.O=S(=O)([O-])C(F)(F)F
trans-{3-[[4-(2-{4-[[3-(dimethylsulfonio)phenyl](phenyl)amino]phenyl}vinyl)phenyl](phenyl)amino]phenl}(dimethyl)sulfonium triflate
C[S+](C)c1cccc(N(c2ccccc2)c2ccc(C=Cc3ccc(N(c4ccccc4)c4cccc([S+](C)C)c4)cc3)cc2)c1.O=S(=O)([O-])C(F)(F)F.O=S(=O)([O-])C(F)(F)F
{3-[[4-(2-{4-[[3-(dimethylsulfonio)phenyl](phenyl)amino]-phenyl}-vinyl)phenyl](phenyl)amino]phenyl}(dimethyl)sulfonium triflate
[F][Sb-]([F])([F])([F])([F])[F].[Na+]
sodium hexafluoroantimonate
C[S+](C)c1cccc(N(c2ccccc2)c2ccc(C=Cc3ccc(N(c4ccccc4)c4cccc([S+](C)C)c4)cc3)cc2)c1.[F][Sb-]([F])([F])([F])([F])[F].[F][Sb-]([F])([F])([F])([F])[F]
{3-[[4-(2-{4-[[3-(dimethylsulfonio)phenyl](phenyl)amino]phenyl}vinyl)phenyl](phenyl)amino]phenyl}(dimethyl)sulfonium hexafluoro-antimonate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他with slow evaporation of methylene chloride and acetone
  2. 2
    其他a yellow solid was formed
  3. 3
    过滤collected by filtration
  4. 4
    洗涤The yellow solid was washed four times with water and three times with ether
  5. 5
    其他NMR-pure product was obtained without further purification in 75.4% (0.31 g)
  6. 6
    其他yield

实验过程

trans-{3-[[4-(2-{4-[[3-(dimethylsulfonio)phenyl](phenyl)amino]phenyl}vinyl)phenyl](phenyl)amino]phenl}(dimethyl)sulfonium triflate (17) (0.3 g 0.33 mmol) was dissolved in methylene chloride (5 ml) and acetone (10 ml). To this solution was added 10 ml aqueous sodium hexafluoroantimonate solution (0.341 g, 1.32 mmol). The resultant mixture was stirred three days in the dark at room temperature with slow evaporation of methylene chloride and acetone, a yellow solid was formed and collected by filtration. The yellow solid was washed four times with water and three times with ether. NMR-pure product was obtained without further purification in 75.4% (0.31 g) yield. 1H NMR (DMSO, 500 MHz) δ ppm: 7.0-7.6 (m, 26H, Ar—H), 7.16 (s, ═CH, 2H), 3.35 (s, CH3, 12H) Anal. calcd for C44H40N2S2Sb2F12: C, 45.51; H, 3.64; N, 2.53; S, 5.78.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07459106B2uspto-grants-2008_12