反应详情

温度

22 °C

Add N-benzyl-2-chloro-N-[(2S)-2-(4-fluorophenyl)-2-hydroxyethyl]acetamide (1440 g, 4.48 mol) to tert-butyl alcohol (14.5 L) and add potassium tert-butoxide (753 g, 6.73 mol) portion-wise while maintaining the mixture at 22° C. Maintain the mixture at 22° C. and stir for 1.5 hours. Add a saturated aqueous solution of ammonium chloride (1306 g) to quench the reaction. Stir for an additional 1 hour and then add H2O (2 L). Extract with EtOAc (2×10 L); combine the extracts; and concentrate the extracts under reduced pressure provide a residue. Re-dissolve the residue in EtOAc (20 L) and wash with H2O (10 L). Dry the EtOAc solution over Na2SO4 and filter. Collect the filtrate and remove the solvent under reduced pressure to provide the title compound as a colorless oil (1250 g, 98%). MS (m/z): 286 (M+1).

1. temperatureMaintain the mixture at 22° C.
2. customto quench
3. customthe reaction
4. stirringStir for an additional 1 hour
5. extractionExtract with EtOAc (2×10 L)
6. concentrationand concentrate the extracts under reduced pressure
7. customprovide a residue
8. washRe-dissolve the residue in EtOAc (20 L) and wash with H2O (10 L)
9. dry with materialDry the EtOAc solution over Na2SO4
10. filtrationfilter
11. customCollect the filtrate
12. customremove the solvent under reduced pressure