反应详情

480 mg of 60% sodium hydride (12.0 mmol) was slowly added to 2.83 g of 5-ethyl-6-(α-cyano-3,5-dimethylbenzyl)-2,4-pyrimidinedione (10.0 mmol) dissolved in 50 ml of dimethyl formamide, and the mixture was stirred at room temperature for one hour. Then, to the resulting solution, 5.07 g of (cyclopent-3-en-1-yl)methyl para-toluenesulfonate (20.0 mmol) was added and stirred with injecting oxygen at 50˜60° C. for 48 hours. After cooling, 200 ml of distilled water was added to the resulting product, and extracted with 200 ml of ethyl acetate (2 ×). The obtained extract was dried with anhydrous magnesium sulfate and concentrated under the reduced pressure. Then, the concentrated residue was separated and purified with column chromatography (hexane:ethyl acetate=2:1) to obtain 2.52 g of the titled compound as a white solid.

1. temperatureAfter cooling
2. extractionextracted with 200 ml of ethyl acetate (2 ×)
3. extractionThe obtained extract
4. dry with materialwas dried with anhydrous magnesium sulfate
5. concentrationconcentrated under the reduced pressure
6. customThen, the concentrated residue was separated
7. custompurified with column chromatography (hexane:ethyl acetate=2:1)