反应详情

0.51 mg of triethylamine and 0.28 ml of acetyl chloride were added under ice-cooling to a solution of 0.77 g of N-(9-fluorenyl)-β-alanine ethyl ester in 25 ml of methylene chloride. The resultant mixture was stirred at 0° C. for 0.5 hour and, then, at room temperature for 3 hours. The reaction solution was poured into ice-cold 1N hydrochloric acid and extracted with methylene chloride. The organic layer was washed with saturated sodium bicarbonate and saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by a silica gel column chromatography (eluting solution: chloroform-methanol) to give 0.85 g of N-acetyl-N-(9-fluorenyl)-β-alanin ethyl ester.

1. extractionextracted with methylene chloride
2. washThe organic layer was washed with saturated sodium bicarbonate and saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by a silica gel column chromatography (eluting solution: chloroform-methanol)