反应详情

Add diethylaminosulfur trifluoride (892 mg, 4 mmol) drop-wise to a solution of (6-fluoro-4-iodo-pyridin-3-yl)-methanol in dichloromethane (25 mL) in a round bottom flask under nitrogen, and then add ethanol (0.3 mL) at 0-5° C. Stir the mixture for 3 hours. Pour the reaction mixture into saturated sodium bicarbonate solution. Abstract the product into chloroform, and wash with water and saturated aqueous sodium chloride. Separate the organic layer from the aqueous layer and dry over MgSO4. After filtration, evaporate the organic solvent in vacuo to give a crude product. Purify the crude with flash column chromatography (10% methanol in dichloromethane) to give the title compound (0.32 g, 53%). MS (ES) m/z 256 [M+1]+.

1. customat 0-5° C
2. washAbstract the product into chloroform, and wash with water and saturated aqueous sodium chloride
3. customSeparate the organic layer from the aqueous layer
4. dry with materialdry over MgSO4
5. filtrationAfter filtration
6. customevaporate the organic solvent in vacuo
7. customto give a crude product
8. customPurify the crude with flash column chromatography (10% methanol in dichloromethane)