反应详情

温度

110 °C

A mixture of (3-[1,3,4]Oxadiazol-2-yl-phenyl)-carbamic acid benzyl ester (200 mg, 0.68 mmol), cyclopropylamine (0.5 mL, 7.2 mmol), trifluoroacetic acid (0.05 mL, 0.65 mmol) in anhydrous 1-butanol (3 mL) was heated at 110° C. overnight in a sealed tube. The reaction mixture was cooled to room temperature and the solvent was removed. The residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution, and the aqueous phase was extracted with ethyl acetate. Solvent was removed after drying with sodium sulfate and purified by silica gel chromatography (rf=0.26 in 20:1 ethyl acetate/methanol) to obtain [3-(4-Cyclopropyl-4H-[1,2,4]triazol-3-yl)-phenyl]-carbamic acid benzyl ester as a white powder (70 mg, 31%). M+1=335.1

1. temperatureThe reaction mixture was cooled to room temperature
2. customthe solvent was removed
3. customThe residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution
4. extractionthe aqueous phase was extracted with ethyl acetate
5. customSolvent was removed
6. dry with materialafter drying with sodium sulfate
7. custompurified by silica gel chromatography (rf=0.26 in 20:1 ethyl acetate/methanol)