反应详情

To a solution of 7-(2-fluoro-4-iodo-phenylamino)-benzo[d]isothiazole-6-carboxylic acid ((R)-2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-amide (263 mg, 0.48 mmol) in MeOH (10 mL) was added a 1.0M aqueous solution of hydrochloric acid (0.97 mL). The reaction mixture was stirred at room temperature for 18 hours before being concentrated in vacuo. The resultant residue was taken up in ethyl acetate, washed with a saturated aqueous solution of sodium hydrogen carbonate then brine, dried (Na2SO4), filtered and evaporated in vacuo. The resultant residue was subjected to flash chromatography (Si—PPC, gradient 0% to 100%, ethyl acetate in DCM) to afford the title compound as a yellow solid (127 mg, 53%). LCMS (method A): RT=9.05 min, [M+H]+=504. 1H NMR (CD3OD, 400 MHz) 8.88 (1 H, s), 7.74 (1 H, d, J=8.36 Hz), 7.61 (1 H, d, J=8.35 Hz), 7.53 (1 H, dd, J=10.01, 1.93 Hz), 7.44 (1 H, ddd, J=8.36, 1.93, 1.06 Hz), 6.76 (1 H, t, J=8.53 Hz), 4.05 (1 H, dd, J=10.03, 3.50 Hz), 3.96-3.83 (2 H, m), 3.63-3.52 (2 H, m).

1. concentrationbefore being concentrated in vacuo
2. washwashed with a saturated aqueous solution of sodium hydrogen carbonate
3. dry with materialbrine, dried (Na2SO4)
4. filtrationfiltered
5. customevaporated in vacuo