反应详情

温度

0 °C

reaction started in ice bath before addition of pivaloyl chloride, then allowed to warm to 23 C, then stirred for ' an additional 6 hours at RT (23 degC)

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 DCM extraction in 1 L separatory funnel · 保留 organic
6. wash未记录说明
7. concentrationrotary evaporator (30 degC, 80 mmHg)
8. dissolution未记录说明
9. flash chromatographyAluminum oxide (neutral, powder, reagent-grade) was purchased from J.T. Baker. The crude reaction mixture is suspended in dichloromethane (50 mL) and is loaded onto a column, with interior diameter of roughly 2 inches, packed with alumina (100 g) and wetted with hexanes. dichloromethane is used as the eluent, and fractions are collected in Erlenmeyer flasks (50 mL each). The desired product typically elutes in fractions 2 through 25. The fractions that contain the desired product are combined
10. concentrationrotary evaporator (30 degC, 80 mmHg)
11. dry in vacuum未记录说明