反应详情

A solution of 3-bromo-5-nitropyridin-4-amine (XLVI) (1 eq.), in neat morpholine in a sealed tube was heated at 120-140° C. overnight. The solution was poured into a mixture of EtOAc and water. The organic layer was separated. The aqueous layer was extracted with EtOAc. The combined organic layers was washed with brine, dried over MgSO4 and concentrated to get a residue. The crude product was purified on a silica gel column eluting with chloroform:MeOH gradient. The fractions containing product were mixed and concentrated under vacuum. The residue was triturated with hexane to give 3-morpholino-5-nitropyridin-4-amine (LIII).

1. customThe organic layer was separated
2. extractionThe aqueous layer was extracted with EtOAc
3. washThe combined organic layers was washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customto get a residue
7. customThe crude product was purified on a silica gel column
8. washeluting with chloroform
9. additionThe fractions containing product
10. additionwere mixed
11. concentrationconcentrated under vacuum
12. customThe residue was triturated with hexane