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General procedure for the selective oxidation of suldes to sulfoxides To a mixture of various suldes (1 mmol) and DBUH-Br3 (0.1 mmol, 0.039 g) in CH3CN (15 mL), H2O2 30% (v/v)(1.4 mmol) was added gradually. After the completion of the reaction which was monitored by TLC using n-hexane:EtOAc (7:3), the solvent was removed and CH2Cl2 (20 mL) was added and the mixture was washed with water(15 mL), 5% HCl solution (15 mL) and water (15 mL), respectively. The organic phase was then dried over anhydrousNa2SO4 and the solvent was removed under reduced pressure. The resulting products were determined by their 1HNMR spectrums and compared with the authentic samples. The synthesis and X-ray structure of DBUH-Br3 as the catalyst have already been reported elsewhere (Fig. 1)[13].In order to get an insight into the optimum catalytic conditions for the selective oxidation of suldes to sulfoxides,the oxidation reaction of methylphenylsulde by hydrogen peroxide as a model experiment was studied at different temperatures and catalyst/H2O2 ratios. The results are summarized in Table 1. Different solvents were also screened. or the oxidation of methylphenylsulde, and as the result acetonitrile was found to be the best solvent in terms of activity and selectivity. |
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至尊木蟲 (職業(yè)作家)
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【答案】應(yīng)助回帖
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sltmac(金幣+1): 謝謝交流~~ 2011-05-30 18:56:52
愚兮兮(金幣+12, 翻譯EPI+1): 2011-05-30 22:01:47
sltmac(金幣+1): 謝謝交流~~ 2011-05-30 18:56:52
愚兮兮(金幣+12, 翻譯EPI+1): 2011-05-30 22:01:47
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General procedure for the selective oxidation of suldes to sulfoxides 選擇性氧化suldes為亞砜的一般步驟 To a mixture of various suldes (1 mmol) and DBUH-Br3 (0.1 mmol, 0.039 g) in CH3CN (15 mL), H2O2 30% (v/v)(1.4 mmol) was added gradually. 向含有不同suldes（1mmol）和DBUH-Br3 (0.1 mmol, 0.039 g)混合物的15mL CH3CN 中逐漸地加入30%(v/v)過氧化氫(1.4 mmol)。After the completion of the reaction which was monitored by TLC using n-hexane:EtOAc (7:3), the solvent was removed and CH2Cl2 (20 mL) was added and the mixture was washed with water(15 mL), 5% HCl solution (15 mL) and water (15 mL), respectively. 反應(yīng)完全（通過正己烷：乙酸乙酯7:3薄層色譜監(jiān)測）后，移除溶劑，加入20mL二氯甲烷，混合液先后分別以15mL水、15mL5%HCl和15mL水清洗。The organic phase was then dried over anhydrousNa2SO4 and the solvent was removed under reduced pressure. 有機(jī)相隨后以無水硫酸鈉干燥并減壓除去溶劑。The resulting products were determined by their 1HNMR spectrums and compared with the authentic samples.產(chǎn)物以氫譜鑒定并和可信樣品對照。 The synthesis and X-ray structure of DBUH-Br3 as the catalyst have already been reported elsewhere (Fig. 1)[13].作為催化劑的DBUH-Br3的合成和X射線衍射結(jié)構(gòu)已有報(bào)道（圖1）。In order to get an insight into the optimum catalytic conditions for the selective oxidation of suldes to sulfoxides,the oxidation reaction of methylphenylsulde by hydrogen peroxide as a model experiment was studied at different temperatures and catalyst/H2O2 ratios. 為了獲得選擇性氧化suldes為亞砜的最佳催化條件，在不同的溫度和催化劑/過氧化氫比條件下，研究了作為模式反應(yīng)的methylphenylsulde 被過氧化氫氧化的反應(yīng)。The results are summarized in Table 1.結(jié)果總結(jié)在表1中。 Different solvents were also screened. 不同的溶劑也進(jìn)行了篩選。For the oxidation of methylphenylsulde, and as the result acetonitrile was found to be the best solvent in terms of activity and selectivity.對methylphenylsulde的氧化，從結(jié)果來看，乙腈就反應(yīng)活性和選擇性而言是最佳溶劑。 |
2樓2011-05-30 09:02:47
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