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A copper acetate‐mediated reaction of benzaldehydes with nitromethane to synthesis of 3‐nitroisoxazoles is reported. A variety of nitro‐aryl‐disubstituted isoxazole derivatives can be prepared in moderate to good yields with benign functional group tolerance. This protocol is successfully applied in gram‐scale reaction. Preliminary mechanistic studies reveal that the aldehyde provided one carbon atom...
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