Sample presentation device
A sample and analyte technology, which is applied in the manufacture and application of sample presentation devices, can solve the problems of increased detection sensitivity and achieve the effect of high-sensitivity detection
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Embodiment I
[0270] Preparation of 11-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyloxy)undec-1-ene (1)
[0271]
[0272] 3.0 mL of 1H,1H,2H,2H-perfluorooctanol (13.7 mmol) was charged into an amber shell vial (40 mL), and 1.4 mL of 50% aqueous potassium hydroxide (13.7 mmol) was added. The solution was heated to 80° C., stirred for 30 minutes, and 3.3 mL of 11-bromoundec-1-ene (1.5 mmol) was added. The reaction was maintained at 80°C for 52 hours until TLC analysis (hexanes) indicated consumption of starting material. The product was cooled to room temperature, added to 100 mL of ethyl acetate, extracted with water (2 x 50 mL) and brine (1 x 50 mL). The ethyl acetate extract was dried over magnesium sulfate, filtered, and the solvent was evaporated in vacuo to give an oily residue. The residue was purified on a silica gel flash column (50 x 300 mm, 0% ethyl acetate / hexane, then 10% ethyl acetate / hexane). Fractions containing the desired product were combined and the solvent was evapo...
Embodiment II
[0274] Preparation of S-[11-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyloxy)undecyl]thioacetate (2)
[0275]
[0276] Into a dry round bottom flask (100 mL) was added 1.0 g of 1 (1.9 mmol) under argon, and 10 mL of anhydrous methanol was added. To the resulting solution was added 426 µL of thioacetic acid (6.0 mmol), followed by 52 mg of 2,2'-azobis(2-methylpropionamidine) dihydrochloride (0.2 mmol). Shield the reaction with aluminum foil and expose it to light from a low-pressure mercury lamp. After 4 hours, TLC analysis (5% ethyl acetate / hexanes) revealed that starting material had been consumed. The solvent was evaporated in vacuo to yield an oily residue. The residue was purified on a silica gel flash column (40 x 300 mm, 0% ethyl acetate / hexane, then 5% ethyl acetate / hexane). Fractions containing the desired product were combined and the solvent was evaporated to yield 856 mg (76%) of 2 as a colorless oil. 1 H NMR (400MHz, CDCl 3 ): δ3.69(t, J=6.8Hz, 2H), 3.43(t...
Embodiment III
[0278] Preparation of 11-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyloxy)undecane-1-thiol (3)
[0279]
[0280] To a brown bottle (20 mL) fitted with a silicon septum with Teflon threads, 850 mg of 2 (1.1 mmol) and 5 mL of 3N methanolic hydrogen chloride (15 mmol) were added. The resulting solution was heated to 40°C for 4 hours. Removal of solvent yielded 782 mg (98%) of 3 as a colorless oil. 1 H NMR (400MHz, CDCl 3 ): δ3.69(t, J=6.8Hz, 2H), 3.43(t, J=6.6Hz, 2H), 2.51(dd, J=7.3, 7.6Hz, 2H), 2.39(m, 2H), 1.58 (m, 4H), 1.32 (t, J=8.0Hz, 1H), 1.25 (width m, 12H).
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