反应详情

温度

80 °C

N-iodo succinimide (35 mg. 0.157 mmol) was dissolved in 3 mL of DMF, and (R)-1-[6-(2,4-Difluoro-phenoxy)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamino]-propan-2-ol (42 mg, 0.131 mmol) was added. The reaction mixture was heated to 80° C. for two hours, after which an additional 35 mg of N-iodo succinimide was added. After heating for two more hours at 80° C., an additional 35 mg of N-iodo succinimide was added. The reaction mixture was heated at 80° C. for 5 more hours, then was cooled to room temperature. The reaction mixture was quenched by addition to water, and was partitioned between water and ethyl acetate. The organic layer was separated, dried over MgSO4, filtered, and evaporated under reduced pressure to give 64 mg of 1-[6-(2,4-Difluoro-phenoxy)-3-iodo-1H-pyrazolo[3,4-d]pyrimidin-4-ylamino]-propan-2-ol. Mass Spec. M+H=448.

1. temperatureAfter heating for two more hours at 80° C.
2. temperatureThe reaction mixture was heated at 80° C. for 5 more hours
3. temperaturewas cooled to room temperature
4. customThe reaction mixture was quenched by addition to water
5. customwas partitioned between water and ethyl acetate
6. customThe organic layer was separated
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. customevaporated under reduced pressure