HRID1644837
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The crude product from step (b) above (1.2 g, 3.83 mmol), 1-(4bromo-benzyl)-1H-imidazole (98.8 mg, 0.416 mmol, see Example 1(d) above), Pd(PPh3)4 (29 mg, 0.25 mmol), NaOH (3 mL, 1M, 3 mmol), toluene (15 mL) and ethanol (3 mL) were mixed under N2 (g). The mixture was heated to reflux for 2 h. The reaction mixture was then diluted with ethyl acetate (150 mL) and washed with water and brine. The organic phase was dried over MgSO4 and the solvent was removed in vacuo. Purification using column chromatography with CHCl3:MeOH (20:1) as eluent yielded the sub-title compound (93.7 mg, 0.220 mmol) in 53% yield.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 2 h
- washwashed with water and brine
- dry with materialThe organic phase was dried over MgSO4
- customthe solvent was removed in vacuo
- customPurification