反应详情

温度

120 °C

To a solution of benzyl 2-(5-(4-bromophenyl)tetrahydro-2H-pyran-2-yl)acetate (300 mg, 0.771 mmol) in dioxane (6 ml) at room temperature was added 4-aminophenylboronic acid (211 mg, 1.541 mmol), Pd(Ph3P)4 (178 mg, 0.154 mmol) and 2M Na2CO3 (1.541 ml, 3.08 mmol) and the mixture was degassed and heated at 120° C. in microwave for 30 min. The reaction was quenched by sat. aq. NH4Cl and was extracted with EtOAc. The combined organic layer was washed with brine and dried over anhydrous sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography (10 to 50% EtOAc (2% TEA)/Heptane) to give the title compound 250 mg (yield 81%). MS (ESI) m/z 402.3 (M+1). Retention time 1.48 min (condition A).

1. customthe mixture was degassed
2. customThe reaction was quenched by sat. aq. NH4Cl
3. extractionwas extracted with EtOAc
4. washThe combined organic layer was washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by flash chromatography (10 to 50% EtOAc (2% TEA)/Heptane)