反应详情

Add (1,3-dioxan-2-ylethyl)magnesium bromide (0.5 M in THF, 40 mL, 20 mmol) to a solution of 2-bromo-4-fluoro-benzaldehyde (3 g, 15 mmol) in THF (20 mL) at 0° C. under N2. Continue to stir the mixture for 48 h at RT. Quench the reaction mixture with 1 N HCl, followed by the basification with diluted ammonium hydroxide to ˜pH 9. Extract the product with chloroform/IPA (3/1). Dry the organic layer over sodium sulfate. Concentrate the solution in vacuo. Purify by column chromatography (10% methanol in DCM) to give the title compound as a yellow oil (24.5 g, 95%). MS (ES) m/z 319/321 [M+1]+.

1. customQuench the reaction mixture with 1 N HCl
2. extractionExtract the product with chloroform/IPA (3/1)
3. dry with materialDry the organic layer over sodium sulfate
4. concentrationConcentrate the solution in vacuo
5. customPurify by column chromatography (10% methanol in DCM)