反应详情

温度

0 °C

Triethylamine (1.5 mL, 11.0 mmol) was added to a mixture of N3-phenylpyridine-2,3-diamine (510 mg, 2.75 mmol), (S)-2-tertbutoxycarbonylaminopropionic acid (0.94 g, 4.96 mmol), HOAt (670 mg, 4.96 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.95 g, 4.96 mmol) in anhydrous DCM (30 mL) at 0° C. under a nitrogen atmosphere. The reaction mixture was stirred at 0° C. for 10 min then slowly warmed to RT. Stirring at RT was continued for 18 h. The reaction mixture was 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, dried (Na2SO4) and concentrated in vacuo to afford the title compound as a light brown foam (1.17 g, quantitative). LCMS (Method C): RT 3.04 min [M+H]+ 357.3.

1. temperaturethen slowly warmed to RT
2. stirringStirring at RT
3. waitwas continued for 18 h
4. customThe reaction mixture was partitioned between DCM
5. extractionThe aqueous phase was further extracted with DCM (×3)
6. washthe combined organic fractions washed with water
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated in vacuo