反应详情

温度

120 °C

A mixture of methyl 2-(bromomethyl)-6-chloroisonicotinate and sodium acetate in N,N-dimethylacetamide is stirred at 120° C. for 2 hours. The mixture is cooled to room temperature and diluted with water (50 mL). The mixture is washed with ethyl acetate/toluene (2:1, 80 mL×2). Water layer is acidified (to pH 4) by the addition of 2M hydrochloric acid, extracted with ethyl acetate (80 mL×2), dried over sodium sulfate. The organic solvent is removed under reduced pressure to give the title compound as a crude product (590 mg, clear brown oil, include N,N-dimethylacetamide). This is used without purification in the next step.

1. temperatureThe mixture is cooled to room temperature
2. washThe mixture is washed with ethyl acetate/toluene (2:1, 80 mL×2)
3. additionby the addition of 2M hydrochloric acid
4. extractionextracted with ethyl acetate (80 mL×2)
5. dry with materialdried over sodium sulfate
6. customThe organic solvent is removed under reduced pressure