反应详情

温度

120 °C

A mixture of D9 (0.2 g, 1.13 mmol), sodium iodide (0.420 g, 2.8 mmol) and hydroiodic acid (57 wt. % in water, 2 ml) was stirred at 120° C. for 10 min., under microwave irradiation. The mixture was then poured into an aqueous saturated solution of sodium carbonate, Na2S2O3, water and dichloromethane. The organic phase was separated, filtered over cotton, and the solvent evaporated in vacuo. The residue was purified by column chromatography (dichloromethane/heptane 1:1 to 8:2) to yield D10 (0.235 g, 77%) as a solid. C6H6ClIN2 requires 268. Found 269 (MH+).

1. customThe organic phase was separated
2. filtrationfiltered over cotton
3. customthe solvent evaporated in vacuo
4. customThe residue was purified by column chromatography (dichloromethane/heptane 1:1 to 8:2)