反应详情

温度

130 °C

A mixture of methyl 5-(bromomethyl)-6-(2,2,2-trifluoroethoxy)nicotinate (0.68 g, 2.07 mmol, Step-2) and sodium acetate (0.51 g, 6.20 mmol) in DMA (10 mL) is stirred at 130° C. for 2 hours. After cooling to room temperature, the reaction mixture is poured into water, extracted with ethyl acetate and dried over sodium sulfate and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-Hexane/ethyl acetate (6:1) to give 0.35 g (56% yield) of the title compound as colorless oil.

1. temperatureAfter cooling to room temperature
2. extractionextracted with ethyl acetate
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 (6:1)