反应详情

温度

100 °C

To a solution of the product obtained in step 1 (1.0 g, 3.70 mmol) in ACN (8 ml) was added CuI (35 mg, 185 μmol), PdCl2(PPh3)2 (389 mg, 554 μmol) and 1-(ethoxyvinyl)tributyl-stannane (2.5 ml, 2.60 g, 7.39 mmol). The mixture was heated for 30 min at 100° C. using microwaves. After cooling, the reaction mixture was acidified with 1 N HCl (4 ml) and stirred for 20 min. The reaction mixture was adjusted to pH=7 using NaHCO3 and extracted with AcOEt. The organic phase was washed with brine, dried over Na2SO4 and evaporated. Purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane (1:1) gave the desired product (650 mg, 75%).

1. temperatureAfter cooling
2. extractionextracted with AcOEt
3. washThe organic phase was washed with brine
4. dry with materialdried over Na2SO4
5. customevaporated
6. customPurification of the crude product by silica gel chromatography