反应详情

To a solution of 4-(2-fluoro-4-iodophenylamino)-indazole-1,5-dicarboxylic acid di-tert-butyl ester (611 mg, 1.10 mmol) in DCM (5 ml) was added TFA (1.2 mL, 16.2 mmol). The reaction mixture was stirred at room temperature for 16 hours before being concentrated in vacuo. The resultant residue was dissolved in ethyl acetate (10 mL), washed with aqueous saturated sodium bicarbonate solution (10 mL) and the aqueous fraction extracted with ethyl acetate (2×10 mL). The combined organic fractions were washed with brine (20 mL), dried (MgSO4) and concentrated in vacuo. The resultant residue was subjected to flash chromatography (Si—PPC, gradient 0-100% ethyl acetate in cyclohexane) to yield the title compound as an off-white solid (367 mg, 84%). LCMS (Method B): RT=3.23 min, [M+H]+=398.

1. concentrationbefore being concentrated in vacuo
2. dissolutionThe resultant residue was dissolved in ethyl acetate (10 mL)
3. washwashed with aqueous saturated sodium bicarbonate solution (10 mL)
4. extractionthe aqueous fraction extracted with ethyl acetate (2×10 mL)
5. washThe combined organic fractions were washed with brine (20 mL)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo