反应详情

温度

40 °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. temperature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. addition未记录说明
6. extraction3 x 50 mL ethyl acetate extraction using a 250-mL separatory funnel · 保留 organic
7. concentrationrotary evaporator (35 degC, 50 mmHg)
8. flash chromatographySilica (30 g) is added to the crude reaction mixture and the solvent removed in vacuo. This mixture 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 1% ethyl acetate in hexanes (2500 mL). During elution, fractions are collected in test tubes (roughly 28 mL each), and the desired product typically elutes around fractions 13 through 72 (Rf = 0.34). The fractions that contain the product are combined.
9. concentrationrotary evaporator (30 degC, 80 mmHg)