反応 #2460317

ord-08cfdb1a527740fcb487f8bf51c29a92

反応方程式

[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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他with slow evaporation of acetone
  2. 2
    その他a yellow solid was formed
  3. 3
    ろ過collected by filtration
  4. 4
    洗浄The yellow solid was washed four times with water and three times with ether
  5. 5
    その他A NMR-pure product was obtained without further purification
  6. 6
    その他isolated in 93.8% (0.95 g)
  7. 7
    その他yield

実験手順

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)

出典

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