反应详情

温度

50 °C

To a solution of the above-mentioned amide compound (157 mg) in benzene (4 mL) was added phosphorus pentachloride (266 mg), and the mixture was stirred at 50° C. for 3 days. After cooling to room temperature, to the reaction mixture was added 2N sodium hydroxide aqueous solution (4 ml), and the reaction mixture was stirred for an additional 30 minutes. The obtained mixture was extracted with chloroform thrice, and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, and the obtained residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=1:1→1:2) to give the objective compound (100 mg).

1. temperatureAfter cooling to room temperature, to the reaction mixture
2. stirringthe reaction mixture was stirred for an additional 30 minutes
3. extractionThe obtained mixture was extracted with chloroform thrice
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated in vacuo
6. customthe obtained residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=1:1→1:2)