反应详情

温度

100 °C

To a solution of 1-(4-methanesulfonyl-phenyl)-4-(piperidin-4-yloxy)-1H-pyrazolo[3,4-d]pyrimidine hydrochloride (30.0 mg, 0.073 m mmol) and Et3N (35 μL) in dioxane (1.5 mL) was added bromomethyl ethyl ketone (22 μL, 0.219 mmol). The mixture was heated by microwave irradiation at 100° C. for 10 min. The mixture was diluted with CH3CN (3 mL) and purified by reverse-phase HPLC: Phenomenex® Luna C18 column (10μ, 250×21.2 mm), 5% (v/v) CH3CN (containing 1% v/v TFA) in H2O (containing 1% v/v TFA) gradient to 95% H2O, 20 mL/min, λ=214 nm to give Compound A168 (7.8 mg, 0.014 mmol, 19% yield) isolated as a white solid. HPLC/MS: Alltech® Prevail C18 column (5μ, 50×4.6 mm), 5% v/v CH3CN (containing 1% v/v TFA) in H2O (containing 1% v/v TFA) gradient to 99% v/v CH3CN in H2O, 3.5 mL/min, tr=1.69 min, ESI+=444.3 (M+H).

1. custompurified by reverse-phase HPLC
2. additionPhenomenex® Luna C18 column (10μ, 250×21.2 mm), 5% (v/v) CH3CN (containing 1% v/v TFA) in H2O (
3. additioncontaining 1% v/v TFA) gradient to 95% H2O, 20 mL/min, λ=214 nm
4. customto give Compound A168 (7.8 mg, 0.014 mmol, 19% yield)
5. customisolated as a white solid