反应详情

A solution of 7-Methoxy-benzo[1,3]dioxole-5-carbaldehyde (I) (1.8 g, 10 mmol) in THF (20 mL) was cooled to −78° C. A solution of methylmagnesium chloride in THF (5.0 mL of 3M, 15 mmol) was added to the solution of i in THF in a dropwise fashion. The reaction was quenched by the addition of HCl (1N, aqueous) and extracted with ethyl acetate. The organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by flash chromatography (silica gel; 40%-60% ethyl acetate in hexanes) to afford 2 (0.89 g, 45%).

1. customThe reaction was quenched by the addition of HCl (1N, aqueous)
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash chromatography (silica gel; 40%-60% ethyl acetate in hexanes)