反应详情

温度

25 °C

To a solution of 4,4,4-trifluoro-2-(4-fluoro-3-methyl-benzenesulfonylamino)-3-trifluoromethyl-butyric acid ethyl ester (29 mg, 0.068 mmol) in anhydrous THF (3 mL) at 0° C. was added 2M LiBH4 (50 μL). The solution was allowed to warm to 25° C. After 18 h, the solution was quenched with 1N HCl and the solvent removed in vacuo. The remaining aqueous phase was transferred to a separatory funnel with distilled water (100 mL) and extracted with EtOAc (100 mL). The organic layer was removed and the aqueous phase extracted with EtOAc (100 mL×2). The organic extracts were combined, washed with brine (100 mL), dried (MgSO4), filtered and evaporated to give a white solid (21 mg). This material was purified by Gilson RP-HPLC (column YMC Combiprep 50×20 mm, gradient 10-100% CH3CN: H2O) to afford a white solid (14 mg, 54%). Mass Spectrum (−ESI): 382 [M−H]−.

1. customthe solution was quenched with 1N HCl
2. customthe solvent removed in vacuo
3. customThe remaining aqueous phase was transferred to a separatory funnel with distilled water (100 mL)
4. extractionextracted with EtOAc (100 mL)
5. customThe organic layer was removed
6. extractionthe aqueous phase extracted with EtOAc (100 mL×2)
7. washwashed with brine (100 mL)
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customevaporated