反应详情

To a solution of 7-(4-bromo-2-fluoro-phenylamino)-benzo[d]isothiazole-6-carboxylic acid (584 mg, 1.59 mmol) and diisopropylethylamine (0.82 mL, 4.77 mmol) in DMF (6 mL) were added O—((R)-2,2-dimethyl-[1,3]dioxolan-4-ylmethyl)-hydroxylamine (468 mg, 3.18 mmol), EDCI (611 mg, 3.18 mmol) and HOBt (430 mg, 3.18 mmol). The reaction mixture was stirred for 18 hours at room temperature, diluted with ethyl acetate, and washed with water, a saturated aqueous solution of sodium hydrogen carbonate then brine before being dried (Na2SO4), filtered and concentrated in vacuo. The resultant residue was subjected to flash chromatography (Si—PPC, gradient 50% to 100%, TBME in cyclohexane) to afford the title compound as a yellow oil (370 mg, 47%). LCMS (method B): RT=3.96 min, [M+H]+=496/498.

1. washwashed with water
2. dry with materiala saturated aqueous solution of sodium hydrogen carbonate then brine before being dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo