反应详情

2—Chloro-6-methyl-3-nitro-N-(1-methoxymethyl-3-methoxypropyl)pyridin-4-amine (˜16.82 mmol) was heated at reflux with Fe powder (10 g) in methanol (120 mL) in the presence of glacial acetic acid (10 mL) for 2 h. Then the iron was filtered through celite, the celite was washed with methanol(80 mL) and the filtrate was stripped in vacuo. The residue was dissolved in 10% HCl (120 mL) and EtOAc was added (160 mL). The mixture was neutralized with solid NaHCO3 and the aqueous layer was extracted with EtOAc (2×100 mL). The combined organic extracts were washed with brine (50 mL), dried (MgSO4) and stripped in vacuo (4.1 g).

1. filtrationThen the iron was filtered through celite
2. washthe celite was washed with methanol(80 mL)
3. dissolutionThe residue was dissolved in 10% HCl (120 mL)
4. additionEtOAc was added (160 mL)
5. extractionthe aqueous layer was extracted with EtOAc (2×100 mL)
6. washThe combined organic extracts were washed with brine (50 mL)
7. dry with materialdried (MgSO4)