HRID1966670

反应详情

EQUATION

反应方程式

HRID 1966670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe solution is cooled
  2. extractionis extracted with H2O (30 mL) and EtOAc (3×15 mL)
  3. dry with materialThe combined organic layer is dried with MgSO4
  4. filtrationis filtered
  5. concentrationThe filtrate is concentrated
  6. customthe residue is purified by silica gel flash column chromatography with 50% EtOAc in heptane as the eluent