反应详情

The above prepared 2,4-Dimethoxy-5-methyl-benzaldehyde (5.40 g, 30 mmol) was dissolved in 150 mL of acetonitrile and treated successively with sodium iodide (6.74 g, 1.5 eq.) and AlCl3 (4.00 g, 1.0 eq.), and the mixture kept at 80° C. for 1 h. Cooling, pouring onto crashed ice, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=9/1), delivered 4.23 g of the title compound as light brown crystals.

1. temperatureCooling
2. additionpouring
3. extractionice, twofold extraction with AcOEt
4. washwashing with water and brine
5. dry with materialdrying over magnesium sulfate, and evaporation of the solvents