反应详情

温度

90 °C

In 36 mL of t-amyl alcohol, 7.3 g of potassium-t-butoxide were solved, and then 10 g of 1-naphthonitrile were added stirring the solution at 90° C. Into the solution, 6.7 mL of diisopropyl succinate were dropped taking time for 2 hours and were placed under reflux for one day. Next, 30 mL of methanol and 4.4 mL of acetic acid were added at 60° C. and then refluxed for 30 minutes. After cooling, the product was separated out through a filter and subsequently rinsed with methanol, thus resulting in a red powder. Next, 2.89 g of the resulting red powder were dissolved in 80 mL of DMF, and 2.1 g of potassium-t-butoxide were added and stirred for one hour. Then, 1.5 mL of methyl iodide was added and stirred at 65° C. for one day. After 50 mL of water was added, extraction was performed with dichloromethane. The extract was concentrated and refined through a column chromatography with silica gel and thus results in 1.5 g of yellow powder. The following is the results of 1H-NMR analysis.

1. customfor 2 hours
2. temperatureunder reflux for one day
3. temperaturerefluxed for 30 minutes
4. temperatureAfter cooling
5. customthe product was separated out through
6. filtrationa filter
7. washsubsequently rinsed with methanol
8. customthus resulting in a red powder
9. stirringstirred for one hour
10. stirringstirred at 65° C. for one day
11. extractionextraction
12. concentrationThe extract was concentrated