反应详情

3-(4-{3-[2-(4-Chloro-phenyl)-2H-indazol-3-yl]-3-cyclohexyl-ureido}-3-fluoro-phenyl)-propionic acid tert-butyl ester (20 mg, 34 μmol) was dissolved in a 4 M solution of HCl in dioxane (190 μl) under an argon atmosphere. The solution was stirred for 14 h at ambient temperature, poured onto ice water/1 N aqueous NaOH solution 1/1 and extracted two times with TBME. The aqueous layer was acidified with 1 N HCl and extracted two times with iPrOAc. The extracts were washed with ice water/brine 1/1 and dried over Na2SO4. The solvent was removed under reduced pressure and the residue was purified by preparative thin layer chromatography (silica gel, CH2Cl2/MeOH) to give the title compound (2 mg, 3.7 μmol; 12%) as yellow foam. MS: m/e=535.3 [M+H+].

1. additionpoured onto ice water/1 N aqueous NaOH solution 1/1
2. extractionextracted two times with TBME
3. extractionextracted two times with iPrOAc
4. washThe extracts were washed with ice water/brine 1/1
5. dry with materialdried over Na2SO4
6. customThe solvent was removed under reduced pressure
7. customthe residue was purified by preparative thin layer chromatography (silica gel, CH2Cl2/MeOH)