反应 #2460317

ord-08cfdb1a527740fcb487f8bf51c29a92

反应方程式

[F][Sb-]([F])([F])([F])([F])[F].[Na+]
sodium hexafluoroantimonate
CCCCc1ccc(N(c2ccc(/C=C/c3ccc(N(c4ccc(CCCC)cc4)c4cccc([S+](C)C)c4)cc3)cc2)c2cccc([S+](C)C)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-(dimethylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl](dimethyl)sulfonium triflate
CCCCc1ccc(N(c2ccc(C=Cc3ccc(N(c4ccc(CCCC)cc4)c4cccc([S+](C)C)c4)cc3)cc2)c2cccc([S+](C)C)c2)cc1.[F][Sb-]([F])([F])([F])([F])[F].[F][Sb-]([F])([F])([F])([F])[F]
[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-(dimethyl-sulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl](dimethyl)sulfonium hexafluoroantimonate

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他with slow evaporation of 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A NMR-pure product was obtained without further purification
  6. 6
    其他isolated in 93.8% (0.95 g)
  7. 7
    其他yield

实验过程

Trans-[3-((4-butylphenyl){4-[2-(4- {(4-butylphenyl)[3-(dimethylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl](dimethyl)sulfonium triflate (19) (0.87 g, 0.83 mmol) was dissolved in acetone (20 ml). To this solution was added 20 ml of an aqueous solution of sodium hexafluoroantimonate (0.88 g, 3.40 mmol). The resultant mixture was stirred two days in the dark at room temperature; with slow evaporation of acetone, a yellow solid was formed and collected by filtration. The yellow solid was washed four times with water and three times with ether. A NMR-pure product was obtained without further purification and isolated in 93.8% (0.95 g) yield. 1H NMR (CD3COCD3, 500 MHz) δ ppm: 7.1-7.4 (m, 24 Ar—H, 2 ═CH), 3.06 (s, 6H, CH3,) 2.72 (t, J=7.7 Hz, CH2, 4H), 1.71 (m, CH2, 4H), 1.46 (m, CH2, 4H), 1.04 (t, J=7.3 Hz, CH3, 6H)

来源

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