反应详情

To a mixture of water (50 mL) and iron powder (3.78 g, 67.7 mmol) at 65° C. was added concentrated hydrochloric acid (1.0 mL) dropwise and the mixture was stirred for 15 min. The aqueous layer of the mixture was poured out and a solution of 2-chloro-N-(2-methyl-1-(naphthalen-2-yl)propan-2-yl)-4-nitroaniline (2.4 g, 6.76 mmol) in THF (50 mL) was added to the above processed iron powder. The mixture was stirred further at 65° C. for 30 min. The mixture was then cooled to rt and filtered, and the filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=8:1) to give the title compound as a white solid (1.86 g, 84%).

1. additionThe aqueous layer of the mixture was poured out
2. stirringThe mixture was stirred further at 65° C. for 30 min
3. filtrationfiltered
4. concentrationthe filtrate was concentrated in vacuo
5. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=8:1)