反应详情

温度

0 °C

To a cold (0° C.) solution of 3-(2-fluoro-4-trimethylsilanyl-phenylamino)-5-formylaminomethyl-pyrazine-2-carboxylic acid methyl ester (480 mg, 1.28 mmol) in dichloromethane (13 mL) under N2 was added dropwise a solution of 1M iodine monochloride in dichloromethane (3.0 mL, 3.0 mmol, 2.4 eq), and the mixture was stirred at 0° C. for 1.5 hour. The reaction was quenched by addition of a saturated aqueous solution of sodium thiosulfate (3 mL). After stirring for 10 minutes the reaction mixture was poured into ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate, water and brine, dried (Na2SO4), filtered and evaporated in vacuo to afford the desired product as a yellow solid (548 mg, 99%). LCMS (method C): RT=2.65 min, [M+H]+=431.

1. customThe reaction was quenched by addition of a saturated aqueous solution of sodium thiosulfate (3 mL)
2. stirringAfter stirring for 10 minutes the reaction mixture
3. additionwas poured into ethyl acetate
4. washThe organic layer was washed with a saturated aqueous solution of sodium bicarbonate, water and brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo