反应详情

温度

75 °C

Stir a solution of 2-cyano-3,5-dimethylpyridine (20.3 g, 0.153 mol) in 100 mL of acetic acid and 20 mL of conc. sulfuric acid over 10 minutes. Add t-butanol (20 ml.) over an additional 15 minutes. Warm the solution to 75° C. and maintain for 30 minutes. Cool to room temperature and basify with 25% NaOH. Extract the product (3X) with ethyl acetate (600 mL). Combine the organic portions and wash (1X) with brine. Dry (Na2SO4), filter and concentrate in vacuo to produce the title compound as a yellowish oil (31.26 g).

1. temperaturemaintain for 30 minutes
2. temperatureCool to room temperature
3. extractionExtract the product (3X) with ethyl acetate (600 mL)
4. washCombine the organic portions and wash (1X) with brine
5. dry with materialDry (Na2SO4)
6. filtrationfilter
7. concentrationconcentrate in vacuo