反应详情

温度

60 °C

To 321 mg (75% w/w, 1.37 mmol) azetidine-1,3-dicarboxylic acid monobenzyl ester in 10 mL dry THF were added 82 mg NaH (2.05 mmol, 60% dispersion in mineral oil), 182 mg 18-crown-6 (0.68 mmol), 328 μL chloroacetone (4.11 mmol), and the mixture was stirred at 60° C. for 6 hours. After cooling to room temperature, 10 mL 1 M sodium bicarbonate was added and the mixture was extracted with DCM (2×10 mL), the organic layers were combined and dried over Na2SO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, heptane-EtOAc 1:1 to EtOAc).

1. temperatureAfter cooling to room temperature
2. extractionthe mixture was extracted with DCM (2×10 mL)
3. dry with materialdried over Na2SO4
4. filtrationAfter filtration and evaporation of the solvent the product
5. customwas purified by column chromatography (silica, heptane-EtOAc 1:1 to EtOAc)