反应详情

To a solution of 5-cyclopropanesulfonylamino-4-(2-fluoro-4-iodo-phenylamino)-indazole-1-carboxylic acid tert-butyl ester (206 mg, 0.36 mmol) in DCM (8 mL) was added TFA (1 mL) and the reaction mixture stirred at room temperature for 2 hours. Additional TFA (1 mL) was added and stirring continued for a further 1 hour before the reaction mixture was concentrated in vacuo and the residue azeotroped with DCM, methanol and then DCM again. The resultant residue was triturated with diethyl ether, the solid filtered off and dried under vacuum at 40° C. to give the title compound as a yellow solid (83 mg, 49%). LCMS (Method A): RT=10.03 [M+H]+=437, 1H NMR (DMSO-d6, 400 MHz): 13.14 (1 H, s), 9.07 (1 H, s), 7.80 (1 H, s), 7.57 (1 H, dd, J=10.84, 1.96 Hz), 7.39 (1 H, s), 7.31 (1 H, d, J=8.74 Hz), 7.25-7.20 (2 H, m), 6.45 (1 H, t, J=8.84 Hz), 2.40-2.32 (1 H, m), 0.75-0.62 (4 H, m), −0.05 (1 H, t, J=3.33 Hz).

1. stirringstirring
2. waitcontinued for a further 1 hour before the reaction mixture
3. concentrationwas concentrated in vacuo
4. customthe residue azeotroped with DCM, methanol
5. customThe resultant residue was triturated with diethyl ether
6. filtrationthe solid filtered off
7. customdried under vacuum at 40° C.