反应详情

温度

60 °C

A solution of methyl 4-chloro-3′,5′-difluoro-6-nitro-5-[(trimethylsilyl)ethynyl]biphenyl-2-carboxylate (4.6 g, 11 mmol) in methanol (46 mL), water (13 mL), and acetic acid (31 mL) was treated with iron (<10 micron) (3.0 g, 54 mmol) and heated at 60° C. for 2 hours. The reaction mixture was treated with additional iron (1.0 g, 18 mmol) and heated at 60° C. for 1 hour to drive the reaction to completion. The reaction mixture was diluted with ethyl acetate (50 mL) and filtered over celite. The filtrate was concentrated to a crude residue. The crude residue was diluted with ethyl acetate and filtered through a short plug of silica gel. The filtrate was concentrated to give the desired product (4.28 g, quantitative). LCMS for C19H19ClF2NO2Si (M+H)+: m/z=394.1; Found: 393.9.

1. temperatureheated at 60° C. for 1 hour
2. customthe reaction to completion
3. filtrationfiltered over celite
4. concentrationThe filtrate was concentrated to a crude residue
5. additionThe crude residue was diluted with ethyl acetate
6. filtrationfiltered through a short plug of silica gel
7. concentrationThe filtrate was concentrated