反应详情

1,3-Dibromo-5-fluoro-2-methoxy-benzene (14.2 g, 50 mmol), phenyl-methanethiol (5.86 ml, 50 mmol), Pd2dba3 (1.145 g, 1.25 mmol, 2.5 mol-%), Xantphos (1.447 g, 2.5 mmol, 5 mol-%) and DIPEA (17.5 ml, 100 mmol) were dissolved in 130 ml dry, degassed 1,4-dioxane and heated to reflux for 3 h. After cooling down the mixture was filtrated and evaporated. The remaining solid (22 g) is chromatographed on silica gel using n-heptane-MTBE as eluent. Yield: 12.42 g, 76%.

1. customdry
2. customdegassed 1,4-dioxane
3. temperatureheated
4. temperatureto reflux for 3 h
5. temperatureAfter cooling down the mixture
6. filtrationwas filtrated
7. customevaporated
8. customThe remaining solid (22 g) is chromatographed on silica gel