反应详情

温度

0 °C

Concentrated H2SO4 (10 ml) was added at 0° C. to a solution of 1-(tert-butoxy-carbonylamino)-cyclobutane-1-carboxylic acid (9.29 mmol, 1 equiv.) in MeOH (30 ml), and the reaction was refluxed for 2 hours at 0° C. The solvent was removed under reduced pressure. The residue was taken up in distilled water, adjusted to pH 8-9 with saturated sodium hydrogen carbonate solution and extracted with ethyl acetate (2×200 ml). The combined organic phases were washed with distilled water (2×150 ml) and saturated NaCl solution (2×50 ml) and dried over sodium sulfate. The solvent was concentrated under reduced pressure to yield the desired product in the form of a white solid. Yield: 75%

1. customThe solvent was removed under reduced pressure
2. extractionextracted with ethyl acetate (2×200 ml)
3. washThe combined organic phases were washed with distilled water (2×150 ml) and saturated NaCl solution (2×50 ml)
4. dry with materialdried over sodium sulfate
5. concentrationThe solvent was concentrated under reduced pressure