反应详情

温度

110 °C

A test tube was charged with CuI (20 mg, 0.10 mmol, 0.10 equiv), 1,10-phenanthroline (36 mg, 0.20 mmol, 0.20 equiv), Cs2CO3 (652 mg, 2.0 mmol, 2.0 equiv), 4-iodoanisole (234 mg, 1.0 mmol, 1.0 equiv), trans-2-buten-1-ol (171 μL, 2.0 mmol, 2.0 equiv) and toluene (0.5 mL). The test tube was sealed and the reaction mixture was stirred at 110° C. for 22 h. The resulting suspension was cooled to room temperature and filtered through a 0.5×1 cm pad of silica gel, eluting with diethyl ether. The filtrate was concentrated in vacuo. Purification of the residue by flash chromatography on silica gel (2×20 cm; pentane:diethyl ether 30:1) provided 153 mg (86% yield) of the title compound as a light yellow oil.

1. customThe test tube was sealed
2. temperatureThe resulting suspension was cooled to room temperature
3. filtrationfiltered through a 0.5×1 cm pad of silica gel
4. washeluting with diethyl ether
5. concentrationThe filtrate was concentrated in vacuo
6. customPurification of the residue by flash chromatography on silica gel (2×20 cm; pentane:diethyl ether 30:1)