反应详情

Cool a solution of 4-benzo[b]thiophen-7-yl-pyridine-3-carbaldehyde (1.5 g, 6.27 mmol in THF (50 mL) in a 250-mL round bottom flask to 0° C. and add gradually methylmagnesium bromide (2.38 g, 6.90 mmol, 2.30 mL) to the solution. Stir the mixture from 0° C. to RT for 2 h. Hydrolyze the mixture by mixing with 1 N HCl (200 mL). Adjust the pH to 11 with ammonium hydroxide. Extract into chloroform/IPA (3/1, 200 mL). Wash the organic phase with water and saturated aqueous sodium chloride. Dry over sodium sulfate and concentrate in vacuo. Purify by FCC (hexane to 10% ethyl acetate in hexane, then 20% THF in DCM) to give the title compound as a yellow oil (1.00 g, 62%). MS (ES) m/z 256 [M+1]+.

1. extractionExtract into chloroform/IPA (3/1, 200 mL)
2. washWash the organic phase with water and saturated aqueous sodium chloride
3. dry with materialDry over sodium sulfate
4. concentrationconcentrate in vacuo
5. customPurify by FCC (hexane to 10% ethyl acetate in hexane