反应详情

温度

110 °C

To a manually stirred polyphosphoric acid (30 g, 200 mmol) in a 200 mL beaker was added 6-methyl-2-pyridinamine (Aldrich, 4.7 g, 43 mmol), followed by methyl 4-chloro-3-oxopentanoate (8.584 g, 52.15 mmol). The mixture was heated with stirring at 110° C. for 5 h. After being cooled, the dark slurry was transferred on to 100 g of ice. The pH of the mixture was adjusted to 6-7 with 10% sodium hydroxide. The mixture was extracted with methylene chloride. The combined organic layers were washed with water, brine, dried over magnesium sulfate and evaporated to dryness. The residue was purified on silica gel, eluting with 0-10% methanol in methylene chloride, to yield the desired product (3.16 g, 32.7%). LCMS calculated for C11H12ClN2O (M+H)+: m/z=223.1. Found: 223.2.

1. temperatureThe mixture was heated
2. temperatureAfter being cooled
3. extractionThe mixture was extracted with methylene chloride
4. washThe combined organic layers were washed with water, brine
5. dry with materialdried over magnesium sulfate
6. customevaporated to dryness
7. customThe residue was purified on silica gel
8. washeluting with 0-10% methanol in methylene chloride