Ethylacetate(Quimis,p.a.),methanol(Quimis,p.a.),sec-butanol(Merck,HPLCgrade),oleicacid(Merck,extrapure),hydrogenperoxide(Interox,70%,w/waqueoussolution),aluminumoxideforc... Ethyl acetate (Quimis, p.a.), methanol (Quimis, p.a.), sec- butanol (Merck, HPLC grade), oleic acid (Merck, extra pure), hydrogen peroxide (Interox, 70%, w/w aqueous solution),
aluminum oxide for chromatography (Fluka, 0.05–0.15 mm), aluminum oxide for column chromatography (Acros Organics, activated, acidic, 0.1–0.5 mm), aluminum tri-sec-butoxide
(Aldrich, 99.99%), oxalic acid (Synth, p.a.), di-n-butyl ether (Fluka, >99%) and soybean oil (Cargill) were used as received. The solution of anhydrous hydrogen peroxide (24%, w/w) in ethyl acetate was prepared from aqueous H2O2 (70%, w/w) in ethyl acetate by azeotropic distillation with a Dean-Stark apparatus [14]
The products were identified by gas chromatography–mass spectroscopy (GC–MS) using a Hewlett-Packard 5890 gas chromatograph equipped with a AT-Wax column and interfaced with a Hewlett-Packard 5971A mass spectrometer. Helium was used as the carrier gas. A similarly equipped Hewlett-Packard5890 gas chromatograph using nitrogen as the carrier gas and a flame ionization detector was used for product quantification, with the help of calibration curves.
Ethyl acetate (Quimis, p.a.), methanol (Quimis, p.a.), sec- butanol (Merck, HPLC grade), oleic acid (Merck, extra pure), hydrogen peroxide (Interox, 70%, w/w aqueous solution),
aluminum oxide for chromatography (Fluka, 0.05–0.15 mm), aluminum oxide for column chromatography (Acros Organics, activated, acidic, 0.1–0.5 mm), aluminum tri-sec-butoxide
(Aldrich, 99.99%), oxalic acid (Synth, p.a.), di-n-butyl ether (Fluka, >99%) and soybean oil (Cargill) were used as received. The solution of anhydrous hydrogen peroxide (24%, w/w) in ethyl acetate was prepared from aqueous H2O2 (70%, w/w) in ethyl acetate by azeotropic distillation with a Dean-Stark apparatus [14].
乙酸乙酯(Quimis,p.a)、甲醇(Quimis,p.a)、仲丁醇(Merck,HPLC等级)、油酸(Merck,超纯)过氧化氢(Interox, 70%,w/w水溶液)、气相色谱用氧化铝(Fluka,0.05-0.15mm)、用于柱层析的氧化铝(Acros Organics,活化的,酸性的,0.1-0.5mm),三-仲丁醇(Aldrich, 99.99%)、草酸(Synth, p.a.)、二-n-丁醚(Fluka,>99.%)和大豆油(Cargill)被采用采纳。无水过氧化氢在乙酸乙酯中的溶液(24%,w/w)由乙酸乙酯中的含水H2O2(70%, w/w)通过用Dean-Stark设备共沸精馏而制备【14】。
The products were identified by gas chromatography–mass spectroscopy (GC–MS) using a Hewlett-Packard 5890 gas chromatograph equipped with a AT-Wax column and interfaced with a Hewlett-Packard 5971A mass spectrometer. Helium was used as the carrier gas. A similarly equipped Hewlett-Packard5890 gas chromatograph using nitrogen as the carrier gas and a flame ionization detector was used for product quantification, with the help of calibration curves.
产品用气相色谱质谱反光镜法(GC-MS)鉴定,用HP公司的5890气相色谱仪配备AT-Wax毛细管柱,并与一台HP公司的5971质谱仪接口。氦被用作载流气体。一台类似配备的HP5890 气体色谱仪采用氮气作为载流气体,一台氢火焰离子化检测器被用于借助校准曲线检验产品的合格与否。