反应详情

温度

-30 °C

N-carbobenzoxy-3-fluoro-4-morpholinylaniline (0.33 g, 1 mmol) was added to 8 mL of methanol. The solution was cooled to −30° C. under the protection of nitrogen flow and then the methanol solution containing 1 mmol of tert-butyl lithium was added. The mixture was stirred at −78° C.˜−20° C. for 2 hours. (S)-1-chloro-3-(dibenzylamino)propan-2-ol (0.29 g, 1 mmol) was added and then the mixture was heated slowly to 100° C. and stirred for 2 hours. After the solution was cooled down, saturated ammonium chloride solution and ethyl acetate were added to separate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, filtered, and evaporated to dryness to provide 0.31 g of white solid in 65% yield. HPLC: 99.2%.

1. additionwas added
2. temperaturethe mixture was heated slowly to 100° C.
3. stirringstirred for 2 hours
4. temperatureAfter the solution was cooled down
5. customto separate
6. washThe organic layer was washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. customevaporated to dryness