反应详情

To a cooled (0° C.) solution of 7-fluoro-3-(2-fluoro-4-trimethylsilanyl-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (1.0 g, 2.48 mmol) in DCM (25 mL) was added iodine monochloride (1M in DCM, 4.96 mmol, 4.96 mL) dropwise. The mixture was stirred cold for 30 minutes then quenched by the addition of a saturated solution of sodium thiosulphate. The organic layer was separated, washed with a saturated solution of sodium thiosulphate, then dried (Na2SO4), filtered and evaporated to give a residue. The residue was triturated with diethyl ether to provide the title compound as a beige solid (805 mg, 71%). LCMS (method B): RT=3.52 min, M+H+ 458.

1. customthen quenched by the addition of a saturated solution of sodium thiosulphate
2. customThe organic layer was separated
3. washwashed with a saturated solution of sodium thiosulphate
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. customto give a residue
8. customThe residue was triturated with diethyl ether