反应详情

温度

80 °C

To 2-Bromothiazole (0.27 mL, 3.0 mmol) in 1,4-dioxane (20 mL) was added iPr2NEt (0.96 mL, 5.5 mmol), and the reaction was degassed with N2 for 10 minutes. 10e (765 mg, 2.8 mmol) was added, followed by Pd2dba3 (63 mg, 0.07 mmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (81 mg, 0.14 mmol). The reaction was sealed and heated overnight at 80° C., and then cooled to room temperature and concentrated. The residue was diluted with EtOAc and water, and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated, and the crude material was purified by silica gel chromatography (60-100% EtOAc in hexanes) to give the desired product, 10f.

1. customthe reaction was degassed with N2 for 10 minutes
2. customThe reaction was sealed
3. temperaturecooled to room temperature
4. concentrationconcentrated
5. additionThe residue was diluted with EtOAc and water
6. extractionthe aqueous layer was extracted with EtOAc
7. dry with materialThe combined organic layers were dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customthe crude material was purified by silica gel chromatography (60-100% EtOAc in hexanes)