Polymeric substrates with fluoroalkoxycarbonyl groups for amine capture
A fluoroalkyl, polymer material technology
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[0141] These examples are illustrative only, and are not intended to limit the scope of the appended claims. All parts, percentages, ratios, etc. in the examples, as well as in the remainder of the specification, are by weight unless otherwise indicated. Solvents and other reagents used were obtained from Sigma-Aldrich Chemical Company, Milwaukee, Wisconsin unless otherwise indicated.
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preparation example 1
[0144] Preparation Example 1: Preparation of Oxyethyl Glutaryl Chloride Monomethacrylate
[0145] A solution of 2-hydroxyethyl methacrylate (57.0 g), glutaric anhydride (50.0 g) and phenothiazine (0.15 g) in dry THF (250 mL) was cooled in a glass reaction vessel with an ice / water bath . Triethylamine (46.0 g in 10 mL THF) was added dropwise to the stirred mixture. The mixture was allowed to warm to room temperature and stirred for 2 days. The solution was concentrated using a rotary evaporator and the remaining mixture was dissolved in CH 2 Cl 2 (250 ml). This solution was washed twice with 150 ml of 5% hydrochloric acid solution and twice with 100 ml of water. After washing, the solution was washed with MgSO 4 Dry, and remove the solvent with a rotary evaporator to yield 105.4 g of oxyethyl glutarate monomethacrylate as a pink liquid. A sample of this oxyethyl glutarate monomethacrylate (50.0 g) was dissolved in CH 2 Cl 2 (100ml). To this was added phenothiazine (...
preparation example 2
[0146] Preparation Example 2: Preparation of Hexafluoroisopropyl Ester of Glutaryl Chloride Monooxyethyl Methacrylate prepare
[0147] Hexafluoroisopropanol (8.6 g), CH 2 Cl 2(50 mL), and ethyldiisopropylamine (5.4 g) were slowly added to the stirred mixture of acid chloride from Preparative Example 1 (10.5 g) over several minutes. The resulting mixture was stirred for 2 hours and the volatiles were removed with a rotary evaporator. The residue was dissolved in methyl tert-butyl ether and filtered through a microfilter. Solvent was removed using a rotary evaporator to give 9.0 grams of oil. The oil was dissolved in hexane (20 mL) and filtered through a microfilter. The solvent was removed using a rotary evaporator to give 8.5 g of a clear beige liquid. The identity of the product was confirmed by proton and fluorine nuclear magnetic resonance (NMR).
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