反应详情

温度

2.5 °C

A solution of 7-fluoro-3-(2-fluoro-4-trimethylsilanyl-phenylamino)-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (500 mg, 1.28 mmol) in CH2Cl2 (15 mL) was cooled to 0-5° C. and treated dropwise with iodine monochloride solution (2.6 mL, 1M in CH2Cl2). The mixture was stirred at 0-5° C. for one hour and then quenched by addition of a saturated aqueous sodium thiosulfate solution (10 mL). The mixture was diluted with water and dichloromethane. The precipitate formed was filtered off, washed with diethyl ether and dried under vacuum at 50° C. to give the title compound as a yellow solid (218 mg, 38%). LCMS (method B): RT=2.87 min, M+H+= 444.

1. customquenched by addition of a saturated aqueous sodium thiosulfate solution (10 mL)
2. additionThe mixture was diluted with water and dichloromethane
3. customThe precipitate formed
4. filtrationwas filtered off
5. washwashed with diethyl ether
6. customdried under vacuum at 50° C.