反应详情

To a solution of 7-(4-bromo-2-fluoro-phenylamino)-benzo[d]isothiazole-6-carboxylic acid ((R)-2,2-dimethyl-[1,3]dioxolan-4-ylmethoxy)-amide (370 mg, 0.75 mmol) in MeOH (4 mL) was added a 1.0M aqueous solution of hydrochloric acid (1.50 mL). The reaction mixture was stirred at room temperature for 2 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%, MeOH in DCM) to afford the title compound as a yellow solid (242 mg, 71%). LCMS (method A): RT=8.80 min, [M+H]+=456/458. 1H NMR (CD3OD, 400 MHz) 8.87 (1 H, s), 7.76-7.70 (1 H, m), 7.61 (1 H, d, J=8.36 Hz), 7.42-7.36 (1 H, m), 7.30-7.25 (1 H, m), 6.95 (1 H, t, J=8.66 Hz), 4.06 (1 H, dd, J=10.08, 3.55 Hz), 3.96-3.83 (2 H, m), 3.64-3.54 (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