反应 #6887
ord-3d1eef909b754b8da0b694cdccfec3a6
反应方程式
溶剂
反应条件
温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1过滤filtered
- 2浓缩The filtrate was concentrated under reduced pressure
- 3洗涤The organic phase was washed with water (3×15 ml)
- 4干燥dried with sodium sulfate
- 5浓缩concentrated under reduced pressure
- 6workup.DISTILLATIONDistillation of the residue under reduced pressure
实验过程
At 0–5° C., propargyl bromide (12.01 g) was added dropwise with stirring to a suspension of 4-methylpiperidine (10.0 g) and potassium carbonate (13.96 g) in dry acetone (80 ml). The mixture was stirred at 50° C. for 6 hours and then filtered. The filtrate was concentrated under reduced pressure and the residue was taken up in dichloromethane. The organic phase was washed with water (3×15 ml), dried with sodium sulfate and concentrated under reduced pressure. Distillation of the residue under reduced pressure gave 12.73 g of an oil of boiling point 60° C./16 mm Hg.