反应详情

温度

2.5 °C

To a solution of the alcohol (95.7 g) from Step 1 in dichloroethane (925 mL) was added pyridine (625 mL) and the mixture was cooled to 0-5° C. Anhydrous p-toluenesulfonic anhydride (105.7 g) was added and the mixture was warmed to room temperature and stirred for 1 hour and then heated to 90° C. for 2 hours. The mixture was cooled, diluted with dichloromethane (1000 mL) and washed with 1N HCl (3×600 mL). The organic layer was washed with brine, dried with sodium sulfate and the solvents were removed in vacuo. The residue was purified by chromatography on SiO2 using ethyl acetate and hexanes in a 1:1 ratio followed by ethyl acetate to yield benzyl [(4S)-2-oxo-1,3-oxazolidin-4-yl]acetate.

1. temperaturethe mixture was warmed to room temperature
2. temperatureheated to 90° C. for 2 hours
3. temperatureThe mixture was cooled
4. washwashed with 1N HCl (3×600 mL)
5. washThe organic layer was washed with brine
6. dry with materialdried with sodium sulfate
7. customthe solvents were removed in vacuo
8. customThe residue was purified by chromatography on SiO2