反应详情

To 1-cyclopropyl-3-(2-fluoro-4-iodo-phenylamino)-1H-pyrrolo[3,2-c]-pyridine-2-carboxylic acid (2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-amide (65.0 mg, 0.12 mmol) in anhydrous methanol (1.8 mL) was added 4 M Hydrogen chloride in 1,4-Dioxane (1.0 mL), and the reaction mixture was stirred at ambient temperature for 17 h. The solvent was removed in vacuo and the residue was redissolved in acetonitrile (2.0 mL) and loaded onto a Phenomenex Strata-X cartridge (5 g). The cartridge was washed with water (10 mL) and methanol (15 ml). The desired product was then eluted using 2M ammonia in MeOH. Methanol was removed in vacuo to give a brown oil, which was purified by HPLC to obtain 3.3 mg (5.5%) of the desired product as the TFA salt. 1H-NMR (500 MHz, MeOD.) δ ppm 8.96 (s, 1H), 8.45 (d, J=6.81 Hz, 1H), 8.18 (d, J=6.77 Hz, 1H), 7.48 (dd, J=10.76 Hz, 1H), 7.28 (d, J=8.50 Hz, 1H), 6.56 (t, J=9.6, 1H), 4.01-3.86 (m, 1H), 3.85-3.75 (m, 2H), 3.75-3.64 (m, 1H), 3.63-3.47 (m, 2H), 1.34-1.29 (m, 2H), 1.09-1.04 (m, 2H); LC-MS (method D): [M+H]+=527.0, RT=3.33 min.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was redissolved in acetonitrile (2.0 mL)
3. washThe cartridge was washed with water (10 mL) and methanol (15 ml)
4. washThe desired product was then eluted
5. customMethanol was removed in vacuo
6. customto give a brown oil, which
7. customwas purified by HPLC