反应详情

To a solution of 1,1-bis(phenylmethyl)-hexahydro-3H-oxazolo[3,4-a]pyrazin-3-one (0.16 g, 0.50 mmol) in tetrahydrofuran (10 mL) were sequentially added triethylamine (0.14 mL) and phenyl chlorocarbonate (0.12 g, 0.75 mmol), and the mixture was stirred at room temperature for 3 hours. To the reaction solution was added water, and the mixture was extracted with ethyl acetate. The extract was washed with a 0.5 M aqueous sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=10:1 to ethyl acetate). The fractions were concentrated, and to the obtained crystals was added diisopropyl ether, collected by filtration and washed with diisopropyl ether to obtain the title compound (0.19 g, yield 85%).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed with a 0.5 M aqueous sodium hydrogen carbonate solution
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=10:1 to ethyl acetate)
6. concentrationThe fractions were concentrated
7. additionto the obtained crystals was added diisopropyl ether
8. filtrationcollected by filtration
9. washwashed with diisopropyl ether