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 N,N-dimethylacetamide (54 mL) is stirred at room temperature for 4 hours. The reaction mixture is poured into water (100 mL) and extracted with n-hexane/ethyl acetate (1:10, 100 mL). The organic layer is washed with water (100 mL), dried over sodium sulfate, and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (5:1) to give 1.14 g (45% yield) of the title compound as colorless oil.

1. extractionextracted with n-hexane/ethyl acetate (1:10, 100 mL)
2. washThe organic layer is washed with water (100 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (5:1)