反应详情

温度

100 °C

To a solution of 4,4,4-trifluoro-2-(triphenyl-λ5-phosphanylidene)-butyric acid ethyl ester (2.0 g, 4.65 mmol) in THF (5 mL) was added 1 mL of trifluoroacetaldehyde hydrate (tech.). The mixture was sealed in a pressure tube and heated at 100° C. for 3.5 h. After cooling to 23° C., the reaction mixture was eluted through a pad of silica gel (100 g) and Na2SO4 with Et2O (100 mL) to remove the by-products triphenylphosphine oxide and water. The eluent was distilled to remove Et2O and to afford the product as a colorless liquid (1.0 g, 86%).

1. customThe mixture was sealed in a pressure tube
2. temperatureAfter cooling to 23° C.
3. washthe reaction mixture was eluted through a pad of silica gel (100 g) and Na2SO4 with Et2O (100 mL)
4. customto remove the by-products triphenylphosphine oxide and water
5. distillationThe eluent was distilled
6. customto remove Et2O