反应详情

温度

85 °C

A mixture of N-bromosuccinimide (464 mg, 2.61 mmol), 2,2′-azobis(2-methylpropionitrile) (16 mg, 0.10 mmol) and methyl 5-methyl-6-(2,2,2-trifluoroethoxy)nicotinate (500 mg, 2.01 mmol, Step-1) in dichloroethane (10 mL) is stirred at 85° C. for 4 hours. After cooling to room temperature, the reaction mixture is poured into water extracted with dichloroethane 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 (10:1) to give 658 mg (>99% yield) of the title compound as colorless oil.

1. temperatureAfter cooling to room temperature
2. extractionextracted with dichloroethane
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 (10:1)