HRID338504

反应详情

EQUATION

反应方程式

HRID 338504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 4-bromo-2-fluorobenzaldehyde (6.1 g, 0.03 mol) and sodium methoxide (1.78 g, 0.033 mol) in dry methanol (60 mL) was stirred at reflux for 16 hours. The methanol was evaporated. The residue was partitioned between DCM and water. The organic layers were dried over sodium sulfate, concentrated in vacuo to give a yellow solid, which was purified by silica gel chromatography (Petroleum ether/EtOAc=20:1 to 10:1) to give the title compound (6.3 g, 97%) as a light yellow solid.

WORKUP

后处理

  1. temperatureat reflux for 16 hours
  2. customThe methanol was evaporated
  3. customThe residue was partitioned between DCM and water
  4. dry with materialThe organic layers were dried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give a yellow solid, which
  7. customwas purified by silica gel chromatography (Petroleum ether/EtOAc=20:1 to 10:1)