反应详情

温度

100 °C

2,6-Dimethyl-4-nitro-pyridine 1-oxide (9.62 g, 57 mmol) is dissolved in AcOH (300 mL) and Fe (powder, 29 g) is added. The mixture is stirred for 1 h at 100° C. The mixture is cooled to r.t. and filtered. The filtercake is thoroughly washed with AcOH and then discarded. The filtrate is evaporated, diluted with water (100 mL), basified with NaOH (1 M, 100 mL), filtered from the formed precipitate and the filtrate is extracted with CHCl3 (10×50 mL). The combined organic extracts are dried (Na2SO4), filtered and evaporated. The residue is crystallized from heptane-CHCl3 to provide the title compound.

1. temperatureThe mixture is cooled to r.t.
2. filtrationfiltered
3. washThe filtercake is thoroughly washed with AcOH
4. customThe filtrate is evaporated
5. additiondiluted with water (100 mL)
6. filtrationfiltered from the formed precipitate
7. extractionthe filtrate is extracted with CHCl3 (10×50 mL)
8. dry with materialThe combined organic extracts are dried (Na2SO4)
9. filtrationfiltered
10. customevaporated
11. customThe residue is crystallized from heptane-CHCl3