反应详情

To a solution of [4-(2-chloro-phenyl)-pyridin-3-yl]-(2,2,2-trifluoro-ethyl)-carbamic acid tert-butyl ester (120 mg, 310 μmol) in CH2Cl2 (2 mL) at 0° C. was added TFA (2 mL). The reaction mixture was stirred at room temperature for 2 hours and then concentrated under vacuum. The residue was extracted with 30 mL 10% aqueous NaHCO3 solution and 30 mL EtOAc. The layers were separated and the aqueous layer was extracted a second time with 30 mL EtOAc. The combined organic layers were washed with 30 mL brine, dried over MgSO4, filtered and concentrated under vacuum. Light yellow solid (79 mg, 89%). MS (ESI): m/z=287.055 [M+H]+.

1. concentrationconcentrated under vacuum
2. extractionThe residue was extracted with 30 mL 10% aqueous NaHCO3 solution and 30 mL EtOAc
3. customThe layers were separated
4. extractionthe aqueous layer was extracted a second time with 30 mL EtOAc
5. washThe combined organic layers were washed with 30 mL brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under vacuum