反应 #2460318

反应方程式

sodium hexafluoroantimonate

trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl)methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium triflate

trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl) methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium triflate

→

trans-[3-((4-butylphenyl){4-[2-(4-{(4-butylphenyl)[3-((benzyl)methylsulfonio)phenyl]amino}phenyl)vinyl]phenyl}amino)phenyl]((benzyl)methyl)sulfonium hexafluoroantimonate

收率 83.2%

溶剂

acetone

acetone

反应条件

后处理

1. 1
   其他the yellow oil that formed
2. 2
   过滤The yellow solid was collected by filtration
3. 3
   洗涤washed four times with water and three times with ether
4. 4
   其他NMR-pure product was obtained without further purification in 83.2% yield (0.85 g)

实验过程

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.

来源