反应详情

温度

0 °C

To a solution of N-{3-[(2,5-dichloropyrimidin-4-yl)amino]phenyl}-1-(3-nitrophenyl)methanesulfonamide (0.060 g, 0.13 mmol) in water (0.1 mL), methanol (0.5 mL) and acetic acid (0.20 mL) was added iron (0.030 g, 0.53 mmol) powder in one batch. The mixture was stirred at 0° C. for 0.5 h. The reaction was mixed with celite, filtered, and the cake was washed with EtOAc. The brown filtrate was concentrated and EtOAc and NaHCO3/water added. Water phase was extracted with EtOAc twice. The organics were combined, dried over Na2SO4 and concentrated to give the desired product as a yellow powder (0.050 g, 89%. LCMS for C17H15Cl2N5O2S (M+H)+: m/z=423.9, 426.0.

1. additionThe reaction was mixed with celite
2. filtrationfiltered
3. washthe cake was washed with EtOAc
4. concentrationThe brown filtrate was concentrated
5. additionEtOAc and NaHCO3/water added
6. extractionWater phase was extracted with EtOAc twice
7. dry with materialdried over Na2SO4
8. concentrationconcentrated