反应详情

6-(2,4-Difluoro-phenoxy)-3-iodo-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-d]pyrimidine (89 mg) was dissolved in 3 mL of MeOH. Aqueous HCl (2 mL, 18.5%) was added, and the mixture was heated to reflux for four hours. The reaction mixture was cooled to room temperature, transferred to a stoppered flask, and heated to 90° C. for w hours. The reaction mixture was evaporated under reduced pressure and the residue was taken up in 12 mL of EtOAc, made basic with 25 mL of 5 N NaOH, wahsed with water, saturated brine, dried over MgSO4, filtered, and evaporated under reduced pressure to yield 26 mg of 6-(2,4-Difluoro-phenoxy)-3-iodo-1H-pyrazolo[3,4-d]pyrimidine. Mass Spec. M+H=373.

1. temperaturethe mixture was heated
2. temperatureto reflux for four hours
3. customtransferred to a stoppered flask
4. temperatureheated to 90° C. for w hours
5. customThe reaction mixture was evaporated under reduced pressure
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated under reduced pressure