Development of Second Generation Gold-Supported Palladium Material with Low-Leaching and Recyclable Characteristics in Aromatic Amination

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• 作者：Mohammad Al-Amin ; Satoshi Arai ; Naoyoki Hoshiya ; Tetsuo Honma ; Yusuke Tamenori ; Takatoshi Sato ; Mami Yokoyama ; Akira Ishii ; Masashi Takeuchi ; Tomohiro Maruko ; Satoshi Shuto ; Mitsuhiro Arisawa
• 刊名：The Journal of Organic Chemistry
• 出版年：2013
• 出版时间：August 2, 2013
• 年：2013
• 卷：78
• 期：15
• 页码：7575-7581
• 全文大小：434K
• 年卷期：v.78,no.15(August 2, 2013)
• ISSN：1520-6904

文摘

An improved process for the preparation of sulfur-modified gold-supported palladium material [SAPd, second generation] is presented. The developed preparation method is safer and generates less heat (aqueous Na₂S₂O₈ and H₂SO₄) for sulfur fixation on a gold surface, and it is superior to the previous method of preparing SAPd (first generation), which requires the use of the more heat-generating and dangerous piranha solution (concentrated H₂SO₄ and 35% H₂O₂) in the sulfur fixation step. This safer and improved preparation method is particularly important for the mass production of SAPd (second generation) for which the catalytic activity was examined in ligand-free Buchwald鈥揌artwig cross-coupling reactions. The catalytic activities were the same between the first and second generation SAPds in aromatic aminations, but the lower palladium leaching properties and safer preparative method of second generation SAPd are a significant improvement over the first generation SAPd.