HRID2108357
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A solution of piperidine (2 mL) and propargyl bromide (80 wt % in toluene, 0.02 mL, 0.19 mmol) was purged with argon for 10 minutes. The solution was treated with 95G (20 mg, 0.04 mmol), CuI (1 mg, 0.008 mmol) and PdCl2(PPh3)2 (3 mg, 0.004 mmol). The reaction mixture was heated to 80° C. for one hour and then concentrated. The residue was purified by flash chromatography (SiO2, 0% to 10% MeOH/CH2Cl2) to afford the desired compound (13 mg, 62%). HPLC tR=3.17 min (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 254 nm). [M+H+]=562.27.
WORKUP
后处理
- concentrationconcentrated
- customThe residue was purified by flash chromatography (SiO2, 0% to 10% MeOH/CH2Cl2)