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有机反应过程 片段翻译
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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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【答案】应助回帖
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sltmac(金币+1): 谢谢交流~~ 2011-05-30 18:56:52
愚兮兮(金币+12, 翻译EPI+1): 2011-05-30 22:01:47
sltmac(金币+1): 谢谢交流~~ 2011-05-30 18:56:52
愚兮兮(金币+12, 翻译EPI+1): 2011-05-30 22:01:47
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General procedure for the selective oxidation of suldes to sulfoxides 选择性氧化suldes为亚砜的一般步骤 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 中逐渐地加入30%(v/v)过氧化氢(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. 反应完全（通过正己烷：乙酸乙酯7:3薄层色谱监测）后，移除溶剂，加入20mL二氯甲烷，混合液先后分别以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. 有机相随后以无水硫酸钠干燥并减压除去溶剂。The resulting products were determined by their 1HNMR spectrums and compared with the authentic samples.产物以氢谱鉴定并和可信样品对照。 The synthesis and X-ray structure of DBUH-Br3 as the catalyst have already been reported elsewhere (Fig. 1)[13].作为催化剂的DBUH-Br3的合成和X射线衍射结构已有报道（图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. 为了获得选择性氧化suldes为亚砜的最佳催化条件，在不同的温度和催化剂/过氧化氢比条件下，研究了作为模式反应的methylphenylsulde 被过氧化氢氧化的反应。The results are summarized in Table 1.结果总结在表1中。 Different solvents were also screened. 不同的溶剂也进行了筛选。For the oxidation of methylphenylsulde, and as the result acetonitrile was found to be the best solvent in terms of activity and selectivity.对methylphenylsulde的氧化，从结果来看，乙腈就反应活性和选择性而言是最佳溶剂。 |
2楼2011-05-30 09:02:47
