反应详情

温度

90 °C

A stirred solution of D3 (40 mg, 150 umole) in toluene (2 ml) at room temperature under argon was treated with 2M trimethylaluminium in toluene (0.15 ml, 300 umole) and maintained for 15 min, then a solution of D7 (57 mg, 200 umole) in toluene (3 ml) was added and the mixture heated at 90° C. for 1 h. The solution was allowed to cool, then added directly to a silica gel column (5 g) and eluted initially with 2% MeOH/DCM to remove high Rf impurities, then with 10% MeOH/DCM to afford the product. This was triturated with Et2O/DCM to afford the title compound as a beige solid (35 mg, 82%).

1. temperaturemaintained for 15 min
2. temperatureto cool
3. additionadded directly to a silica gel column (5 g)
4. washeluted initially with 2% MeOH/DCM
5. customto remove high Rf impurities
6. customwith 10% MeOH/DCM to afford the product
7. customThis was triturated with Et2O/DCM