反应详情

温度

5 °C

9.75 g (0.22 mol) of sodium hydride (55 percent in oil) was added in 10 portions in 2 hours at -10° C. under argon to a solution of 50.0 g (0.2 mol) of (3aS,6aR)-1-[(R)-(1-phenylethyl)]-dihydro-1H-furo-[3,4-d]-imidazol-2,4(3H,3aH)-dione and 39.8 g (0.25 mol) of 4-methoxybenzyl chloride in 500 ml of dried N,N-dimethylformamide. The reaction mixture was stirred at 5° C. for 2 hours and then at room temperature for another 2 hours. Then 8 ml of acetic acid was added. Then the mixture was evaporated to dryness. Then the residue was taken up in 100 ml of water and 200 ml of dichloromethane, the phases were separated and the aqueous phase was extracted twice with 100 ml of dichloromethane. The organic phases were dried over magnesium sulfate and concentrated. After suspension in ethanol with refluxing, cooling and filtering, 53.5 g (72 percent) of the title product was obtained in the form of white needles. Concerning the product:

1. waitat room temperature for another 2 hours
2. customThen the mixture was evaporated to dryness
3. custom200 ml of dichloromethane, the phases were separated
4. extractionthe aqueous phase was extracted twice with 100 ml of dichloromethane
5. dry with materialThe organic phases were dried over magnesium sulfate
6. concentrationconcentrated
7. temperatureAfter suspension in ethanol with refluxing
8. temperaturecooling
9. filtrationfiltering