反应详情

To a solution of N,N′-carbonyldiimidazole (530 mg, 3.27 mmol in THF (5 mL) was added slowly a solution of 2-amino-3-fluoro-3-methylbutan-1-ol (360 mg, 2.97 mmol) in THF (10 mL). The reaction mixture was stirred at room temperature for 18 hr, was diluted with DCM and stirred for additional 30 min. The separated organic layer was washed with water and brine, dried over sodium sulfate, filtered off and concentrated under reduced pressure. The residue was purified by column chromatography [SiO2, 12 g, EtOAc/heptane=0/100 to 80/20] to provide 4-(2-fluoropropan-2-yl)oxazolidin-2-one (150 mg) as a brown solid. MS m/z 148.0 (M+H)+; Rt-0.32 min. 1H NMR (400 Mhz, CDCl3) δ ppm 6.30 (br. s., 1H), 4.39-4.54 (m, 1H), 4.26 (dd, J=8.9, 5.1 Hz, 1H), 3.84-3.99 (m, 1H), 1.29-1.45 (m, 6H).

1. stirringstirred for additional 30 min
2. washThe separated organic layer was washed with water and brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered off
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography [SiO2, 12 g, EtOAc/heptane=0/100 to 80/20]