反应详情

A solution of 6-9 (0.09 g, 0.142 mmol) in CH2Cl2 cooled to 0° was treated with TMSBr (0.054, 0.355 mmol) and the resulting solution was stirred at rt for 16 hours with cooling. Et2N (100 μl) was added and the solvent was removed. The residue was dissolved in 10% aqueous acetone (5 ml), concentrated, and suspended in toluene to give a solid. This was purified by flash chromatography on silica gel eluting with 10:1:1 EtOH/H2O/NH4OH to give pure 6-10.

1. temperaturewith cooling
2. additionEt2N (100 μl) was added
3. customthe solvent was removed
4. dissolutionThe residue was dissolved in 10% aqueous acetone (5 ml)
5. concentrationconcentrated
6. customto give a solid
7. customThis was purified by flash chromatography on silica gel eluting with 10:1:1 EtOH/H2O/NH4OH
8. customto give pure 6-10