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2 (18 mg, 0.031 mmol), dppp (13 mg, 0.032 mmol). 1,10-phenanthroline (10 mg, 0.055 mmol), and DMF (5 mL). A pressure head was attached; the reaction mixture was pressurized to 6 atm of carbon monoxide and heated at 70 °C for 4 h. A slow change in color from deep purple to brown was observed. Extractive workup with dichloromethane and brine followed by flash chromatography (98:2, hexanes:ethyl acetate) gave 57% of 4b and 40% of 5b.
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