反应详情

To a stirred solution of N-methoxy-N-methyl-6-(2,2,2-trifluoroethoxy)nicotinamide (6.54 g, 24.8 mmol, Step-2) in THF (80 mL) is added dropwise 1.06M methylmagnesium bromide (46.7 mL, 49.5 mmol) at 0° C. The reaction mixture is stirred at rt for 1.5 hours. The reaction mixture is poured into saturated aqueous sodium hydrogen carbonate (100 mL) and extracted with EtOAc (300 mL). The organic layer is washed with water (100 mL×2) and dried over sodium sulfate. After filtration, the filtrate is concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (1:1) to give 4.51 g (83% yield) of the title compound as colorless oil.

1. extractionextracted with EtOAc (300 mL)
2. washThe organic layer is washed with water (100 mL×2)
3. dry with materialdried over sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate is concentrated in vacuo
6. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (1:1)