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3 (150 mg, 1.5 mmol), evacuated, and back-filled with argon. 2-Chloroacetophenone (154 mg, 0.13 mL, 1 mmol) and methylhydrazine (0.35 mL, 6.4 mmol) were added under argon. The Schlenk tube was sealed, and the reaction was stirred magnetically at 110°C for 20 h. The resulting suspension was cooled to room temperature, filtered, diluted with ethyl acetate, and washed with water. The organic phase was concentrated. Purification of the residue by flash cromatography on silica gel (hexane/EtOAc, 95:5) gave the desired product.
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3 (150 mg, 1.5 mmol), evacuated, and back-filled with argon. 2-Chloroacetophenone (154 mg, 0.13 mL, 1 mmol) and methylhydrazine (0.35 mL, 6.4 mmol) were added under argon. The Schlenk tube was sealed, and the reaction was stirred magnetically at 110°C for 20 h. The resulting suspension was cooled to room temperature, filtered, diluted with ethyl acetate, and washed with water. The organic phase was concentrated. Purification of the residue by flash cromatography on silica gel (hexane/EtOAc, 95:5) gave the desired product.
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