反应详情

To a suspension of sodium hydride (0.24 g; 10.0 mmol) in tetrahydrofuran (100 ml) was added 4,4-dimethyloxazolidin-2-one (1.15 g; 10.0 mmol) at 0° C., and the resultant suspension was stirred at room temperature for 5 hours. To the gelatinous reaction mixture was added 2-bromopropionyl bromide (1.05 ml) at 0° C. After stirring for 1 hour, a saturated aqueous solution of potassium dihydrogen phosphate was added to quench the reaction. An aqueous layer was extracted with ethyl acetate. Combined organic layers were dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give a solid residue, which was purified by silica gel column chromatography (hexane:dichloromethane=1:1~0:1) to give 3-(2'-bromopropionyl)-4,4-dimethyloxazolidin-2-one (2.35 g, yield, 90%) as colorless crystals.

1. customto quench
2. customthe reaction
3. extractionAn aqueous layer was extracted with ethyl acetate
4. dry with materialCombined organic layers were dried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customto give a solid residue, which
7. customwas purified by silica gel column chromatography (hexane:dichloromethane=1:1~0:1)