反应详情

温度

45 °C

A stirred mixture of 2-(phenylsulfonylmethyl)-1-nitrobenzene (5.55 g, 20.0 mmol) and granular tin (10.4 g, 88 mmol) in methanol and concentrated HCl (60 mL) is stirred under nitrogen at 45° C. for 5 h, cooled to ambient temperature over an 18 h period, poured onto NaHCO3 (80 g) with stirring, treated with water and extracted with ethyl acetate. The combined extracts are washed with brine (2×100 mL), dried over MgSO4, and concentrated in vacuo to afford the title product as an off-white solid, 4.41 g (89%) mp 175-176° C., identified by HNMR and mass spectral analyses.

1. temperaturecooled to ambient temperature over an 18 h period
2. additionpoured onto NaHCO3 (80 g)
3. stirringwith stirring
4. extractionextracted with ethyl acetate
5. washThe combined extracts are washed with brine (2×100 mL)
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo