反应详情

{2-Chloro-4-[5-[(5-iodo-pyridine-3-carbonyl)-amino]-2-(2,2,2-trifluoro-ethoxy)-pyridin-3-yl]-phenyl}-carbamic acid benzyl ester (87 mg, 127 μmol) was, with cooling, combined with trifluoroacetic acid (3 mL) to give a brown solution. The reaction mixture was warmed to room temperature and stirred for 72 h. The crude reaction mixture was concentrated in vacuo, poured into 50 mL ethyl acetate and extracted with 1 M NaOH (1×25 mL). The aqueous layer was washed with ethyl acetate (1×50 mL). The organic layers were combined, dried with Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 20 g, 0% to 40% EtOAc in heptane) to give the title compound (59 mg, 84%); LC-MS (UV peak area/ESI) 98.1%, 548.9795 (M+H)+.

1. temperaturewith cooling
2. customto give a brown solution
3. customThe crude reaction mixture
4. concentrationwas concentrated in vacuo
5. additionpoured into 50 mL ethyl acetate
6. extractionextracted with 1 M NaOH (1×25 mL)
7. washThe aqueous layer was washed with ethyl acetate (1×50 mL)
8. dry with materialdried with Na2SO4
9. concentrationconcentrated in vacuo
10. customThe crude material was purified by flash chromatography (silica gel, 20 g, 0% to 40% EtOAc in heptane)