反应详情

温度

100 °C

73 mg of tert-butyl (5-bromopyridin-2-yl)carbamate was dissolved in 1 ml of DMF. 62 mg of silver (I) oxide and 31 mg of tetrakis(triphenylphosphine)palladium were added to the obtained solution, and they were stirred at 100° C. in argon atmosphere for 5 minutes. 1 ml of a solution of 100 mg of ethyl 1-cyclopropyl-9-methyl-4-oxo-8-tributylstannyl-4H-quinolizine-3-carboxylate in DMF was added dropwise to the reaction mixture, and they were stirred at that temperature for 1 hour. The reaction mixture was poured into water. After the extraction with chloroform, the organic layer was washed with water and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by the silica gel column chromatography (eluent: hexane/ethyl acetate=1/1) to obtain 11 mg of ethyl 8-(6-tert-butoxycarbonylaminopyridin-3-yl)-1-cyclopropyl-9-methyl-4-oxo-4H-quinolizine-3-carboxylate.

1. stirringwere stirred at that temperature for 1 hour
2. extractionAfter the extraction with chloroform
3. washthe organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe obtained residue was purified by the silica gel column chromatography (eluent: hexane/ethyl acetate=1/1)