反应详情

In 20 ml of methanol was dissolved 1.32 g of 85% potassium hydroxide, and then 3.89 g of 5-chloro-2-methylindan-1,3-dione, 3.76 g of 6-chloro-2-(1-chloromethylvinyl)pyridine and 0.05 g of potassium iodide were added to the solution. After refluxing under heating for 3 hours, the solvent was evaporated and water was poured. The reaction mixture was extracted with ethyl acetate, the organic layer was washed with water and with a saturated saline solution, and then dried over anhydrous magnesium sulfate. After the solvent was evaporated, the residue was separated and purified by silica gel column chromatography (developing solvent: n-hexane/ethyl acetate=5/1) to obtain 6.02 g of the compound No. 115 shown in Table 1.

1. temperatureAfter refluxing
2. temperatureunder heating for 3 hours
3. customthe solvent was evaporated
4. additionwater was poured
5. extractionThe reaction mixture was extracted with ethyl acetate
6. washthe organic layer was washed with water and with a saturated saline solution
7. dry with materialdried over anhydrous magnesium sulfate
8. customAfter the solvent was evaporated
9. customthe residue was separated
10. custompurified by silica gel column chromatography (developing solvent: n-hexane/ethyl acetate=5/1)