反应详情

温度

22 °C

To a solution of 4-iodo-1-methyl-2-nitro-benzene (25.0 g, 107 mmol) in 300 mL of ethanol was added sulfided platinum (3.00 g) and ammonium formate (20.3 g, 321 mmol). The mixture was heated to reflux for 12 h and then cooled to 22° C., filtered through Celite® and concentrated in vacuo. The resulting residue was diluted with H2O (300 mL) and extracted with 3×200 mL CH2Cl2. The organic fractions were combined, washed with brine, dried over Na2SO4 and concentrated in vacuo to give b (21.1 g, 95%): MS m/z=234 (M+H).

1. temperatureThe mixture was heated
2. temperatureto reflux for 12 h
3. filtrationfiltered through Celite®
4. concentrationconcentrated in vacuo
5. additionThe resulting residue was diluted with H2O (300 mL)
6. extractionextracted with 3×200 mL CH2Cl2
7. washwashed with brine
8. dry with materialdried over Na2SO4
9. concentrationconcentrated in vacuo
10. customto give b (21.1 g, 95%)