反应详情

温度

100 °C

In argon atmosphere, a mixture of 34.6 g (105 mmol) of 4-bromo-6-(cyclohexylmethyl)-1,2,3,5-tetrahydro-s-indacene, 22.4 g (126 mmol) 4-tert-butylphenylboronic acid, 66.8 g (315 mmol) of K3PO4, 1.21 g (21 mmol) of Pd(dba)2, 1.73 g (42 mmol) of dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine and 350 ml of toluene was stirred for 12 h at 100° C. The resulting mixture was cooled to room temperature, and then 600 ml of water was added. The organic layer was separated, and the aqueous layer was extracted with 3×100 ml of dichloromethane. The combined organic extract was dried over Na2SO4 and then evaporated to dryness. The target product was isolated by flash chromatography on silica gel 60 (40-63 um; eluent: hexanes). Yield 24.0 g (62%).

1. temperatureThe resulting mixture was cooled to room temperature
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with 3×100 ml of dichloromethane
4. extractionThe combined organic extract
5. dry with materialwas dried over Na2SO4
6. customevaporated to dryness
7. customThe target product was isolated by flash chromatography on silica gel 60 (40-63 um; eluent: hexanes)