反应详情

A mixture of 6-(2,2,2-trifluoroethoxy)picolinic acid (2.40 g, 10.9 mmol, Step-1), methyl iodide (3.39 mL, 54.3 mmol) and potassium carbonate (4.50 g, 32.6 mmol) in DMA (54 mL) is stirred at rt for 4 hours. The reaction mixture is poured into water (100 mL) and extracted with n-hexane/EtOAc (1:10, 100 mL). The organic layer is washed with water (100 mL), 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 (5:1) to give 1.14 g (45% yield) of the title compound as colorless oil.

1. extractionextracted with n-hexane/EtOAc (1:10, 100 mL)
2. washThe organic layer is washed with water (100 mL)
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 (5:1)