反应详情

温度

100 °C

Cesium carbonate (214 mg), pyrrole (30 mg), Xantphos (63 mg), and Pd2(dba)3 (50 mg) were added to a 1,4-dioxane solution (5 mL) containing tert-butyl(5-bromopyridin-3-yl)carbamate (100 mg) in a nitrogen atmosphere, followed by stirring at 100° C. for 8 hours. The reaction solution was adjusted to room temperature, and water was added, followed by extraction with ethyl acetate. The organic layer was washed with saturated saline and dried over anhydrous sodium sulfate. Then, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=5:1 to 1:1), and a light yellow solid of tert-butyl(5-(1H-pyrrol-1-yl)pyridin-3-yl)carbamate (36 mg) was thus obtained.

1. customwas adjusted to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with saturated saline
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThen, the solvent was distilled away under reduced pressure
6. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=5:1 to 1:1)