反应详情

3-(2-Fluoro-4-iodo-phenylamino)-thieno[3,2-c]pyridine-2-carboxylic acid ((R)-2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-amide (18 mg, 0.03 mmol) was dissolved in methanol (1 ml) and concentrated hydrochloric acid (1 drop) added. The mixture was allowed to stir for 2 hours then evaporated to dryness to give a residue. The residue was partitioned between aqueous saturated NaHCO3 solution (10 ml), water (20 ml) and DCM (20 ml). The organic layer was separated, dried over sodium sulphate, filtered and evaporated to give a yellow solid. The solid was purified by flash chromatography (Si-SPE, DCM:MeOH, gradient 98:2 to 92:8) to afford the title compound as a yellow solid (8 mg, 50%). LCMS (method A): RT=6.32 min, M+H+=504. 1H NMR (d4-MeOH, 400 MHz) 8.56 (s, 1H), 8.34 (d, J=5.7 Hz, 1H), 7.87 (d, J=5.7 Hz, 1H), 7.45 (dd, J=10.5 Hz, 1.8 Hz, 1H), 7.27 (d, J=8.5 Hz, 1H), 6.61 (dd, J=8.5 Hz, 8.5 Hz, 1H), 3.89-3.94 (m, 1H), 3.76-3.85 (m, 2H), 3.45-3.54 (m, 2H).

1. customthen evaporated to dryness
2. customto give a residue
3. customThe residue was partitioned between aqueous saturated NaHCO3 solution (10 ml), water (20 ml) and DCM (20 ml)
4. customThe organic layer was separated
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. customevaporated
8. customto give a yellow solid
9. customThe solid was purified by flash chromatography (Si-SPE, DCM:MeOH, gradient 98:2 to 92:8)