反应详情

温度

23 °C

After dropwise addition of dimethoxy(methyl)- silane into reaction mixture in water bath, the vessel was removed and allowed to stir for an additional 12 hours

1. addition未记录说明
2. addition未记录说明
3. addition未记录说明
4. addition未记录说明
5. extraction3 x 50 mL ethyl acetate extraction · 保留 organic
6. concentrationrotary evaporator (35 degC, 50 mmHg)
7. flash chromatographyThe crude reaction mixture is dissolved in a minimal quantity of benzene or toluene and is loaded onto a column, with interior diameter of roughly 2 inches, packed with silica (200 g, SiliCycle, F60/230-400 mesh) and equilibrated with hexanes. The column is eluted under air pressure with hexanes (500 mL), then 1% ethyl acetate in hexanes (1 L), then 2% ethyl acetate in hexanes (1 L). During elution, fractions are collected in test tubes (roughly 28 mL each), and the desired product typically elutes around fractions 18 through 66. The fractions that contain the productare combined
8. concentrationrotary evaporator (30 degC, 80 mmHg)