反应详情

温度

75 °C

A mixture of [(S)-1-(3-phenylaminopyridin-2-ylcarbamoyl)ethyl]carbamic acid tert-butyl ester (980 mg, 2.75 mmol) in AcOH (25 mL) was heated for 10 h at 75° C. under a nitrogen atmosphere. The volatiles were removed in vacuo and the resulting residue partitioned between DCM and a saturated aqueous solution of NaHCO3. The aqueous phase was further extracted with DCM (×3) and the combined organic fractions washed with water, followed by brine, then dried (Na2SO4) and concentrated in vacuo to afford the title compound as a light brown foam (920 mg, 99%). LCMS (Method C): RT 2.88 min [M+H]+ 339.3.

1. customThe volatiles were removed in vacuo
2. customthe resulting residue partitioned between DCM
3. extractionThe aqueous phase was further extracted with DCM (×3)
4. washthe combined organic fractions washed with water
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo