反应详情

To a solution of 2-iodo-1-(methyloxy)-3-[(2-methyl-2-propen-1-yl)oxy]benzene (Intermediate 4, 6.08 g) in toluene (50 ml, SCRC) were added AIBN (3.61 g, 21.99 mmol, SCRC) and tributylstannane (11.60 g, 40.0 mmol, Aldrich). The reaction mixture was heated at reflux for 3 hours and then cooled to room temperature. Water (100 ml) was added and the mixture was extracted with ethyl acetate (3 times 200 ml, SCRC). The combined organic layers were dried, evaporated and purified by silica gel chromatography with as eluents EtOAc/PE (1/50) to afford the title compound as a yellow liquid (2.7 g).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3 hours
3. extractionthe mixture was extracted with ethyl acetate (3 times 200 ml, SCRC)
4. customThe combined organic layers were dried
5. customevaporated
6. custompurified by silica gel chromatography with as eluents EtOAc/PE (1/50)