反应详情

A mixture of 2-(bromomethyl)-1-chloro-3-iodobenzene (14 g, 42 mmol) in 100 mL EtOH was treated with a solution of potassium cyanide (3.6 mL, 84 mmol) in 40 mL water. The mixture was refluxed for 2.5 hours. The mixture was cooled to room temperature and then concentrated. The residue was diluted with 200 mL EtOAc, washed with water (2×50 mL), saturated NaCl (50 mL), dried over sodium sulfate and concentrated. The crude product was purified by column chromatography (20% EtOAc/hexane) to give 10.18 g pale yellow solid. MS m/e: (M−1)− 276.

1. temperatureThe mixture was refluxed for 2.5 hours
2. concentrationconcentrated
3. additionThe residue was diluted with 200 mL EtOAc
4. washwashed with water (2×50 mL), saturated NaCl (50 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe crude product was purified by column chromatography (20% EtOAc/hexane)