反应详情

In 20 ml of anhydrous tetrahydrofuran was suspended 191 mg of (4R)-2-oxo-4-thiazolidinecarboxylic acid and 294 mg of trans-4-(2-nitroxyethyl)cyclohexylmethylamine hydrochloride, and 0.54 ml of triethylamine and 0.28 ml of diphenylphosphoric azide were added thereto with stirring under ice-cooling, and the resulting mixture was stirred at room temperature for 4 hours. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluting solvent: cyclohexane/ethyl acetate=1/3) and recrystallizated from dichloromethane-diisopropyl ether to obtain 200 mg of the desired compound as a colorless crystalline solid.

1. additionwere added
2. temperaturecooling
3. stirringthe resulting mixture was stirred at room temperature for 4 hours
4. distillationThe solvent was distilled off under reduced pressure
5. customthe residue was purified by silica gel column chromatography (eluting solvent: cyclohexane/ethyl acetate=1/3)