反应详情

温度

0 °C

To a cooled (0° C.) solution of 7-fluoro-3-(2-fluoro-4-trimethylsilanyl-phenylamino)-thieno[3,2-c]pyridine-2-carboxylic acid ethyl ester (330 mg, 0.81 mmol) in DCM (10 mL) was added iodine monochloride (1M in DCM, 1.6 mL, 1.6 mmol) dropwise. On complete addition the mixture was allowed to stir at 0° C. for 1 hour then quenched by the addition of saturated sodium thiosulphate solution (10 mL). The mixture was stirred vigorously for 10 min and partitioned between ethyl acetate and water. The organic layer was separated and washed with a saturated solution of sodium hydrogenocarbonate followed by brine, dried over sodium sulphate, filtered and concentrated to give the title compound as a yellow solid (358 mg, 54%). LCMS (method B): RT=4.72 min, M+H+=461.

1. additionOn complete addition the mixture
2. customthen quenched by the addition of saturated sodium thiosulphate solution (10 mL)
3. stirringThe mixture was stirred vigorously for 10 min
4. custompartitioned between ethyl acetate and water
5. customThe organic layer was separated
6. washwashed with a saturated solution of sodium hydrogenocarbonate
7. dry with materialdried over sodium sulphate
8. filtrationfiltered
9. concentrationconcentrated