反应详情

温度

60 °C

A mixture of tert-butyl [5-({2-[(tert-butoxycarbonyl)amino]-5-nitrophenyl}ethynyl)pyridin-3-yl]carbamate (1.60 g, 3.52 mmol), methanol (37 mL), acetic acid (7.3 mL), water (3.7 mL) and iron (905 mg, 16.2 mmol) was stirred at 60° C. for 3 h. The reaction mixture was filtered through a pad of celite and washed with ethyl acetate and extracted with ethyl acetate once. The combined organic solutions were dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by flash column chromatography to yield the desired product (1.40 g, 94%). LCMS calculated for C23H29N4O4(M+H)+: m/z=425.1.

1. filtrationThe reaction mixture was filtered through a pad of celite
2. washwashed with ethyl acetate
3. extractionextracted with ethyl acetate once
4. dry with materialThe combined organic solutions were dried with sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by flash column chromatography