HRID1966670
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
- 100 °C
PROCEDURE
实验过程
To a solution of 2-fluoro-5-methoxybenzaldehyde (200 mg, 1.29 mmol) in DMSO (10 mL) are added 1,2,4-triazole (134 mg, 1.95 mmol) and K2CO3 (359 mg, 2.60 mmol) at room temperature. The solution is heated to 100° C. for 2 hours. The solution is cooled and is extracted with H2O (30 mL) and EtOAc (3×15 mL). The combined organic layer is dried with MgSO4 and is filtered. The filtrate is concentrated and the residue is purified by silica gel flash column chromatography with 50% EtOAc in heptane as the eluent to afford 5-methoxy-2-1,2,4-triazol-1-yl-benzaldehyde (53 mg, 20%) as a white foam.
WORKUP
后处理
- temperatureThe solution is cooled
- extractionis extracted with H2O (30 mL) and EtOAc (3×15 mL)
- dry with materialThe combined organic layer is dried with MgSO4
- filtrationis filtered
- concentrationThe filtrate is concentrated
- customthe residue is purified by silica gel flash column chromatography with 50% EtOAc in heptane as the eluent