反应详情

To a solution of di(1H-imidazole-1-yl)methanamine (1.05 g, 6.52 mmol) in THF (30 mL) was added methyl-2-amino-5-fluoro-3-hydroxybenzoate (0.96 g, 5.22 mmol) at room temperature and the resulting reaction mixture was heated to reflux for 6 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The residue was dissolved in EtOAc (200 mL) and washed with H2O (4×100 mL), saturated aqueous ammonium chloride (2×100 mL), brine (2×100 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure to afford methyl 2-amino-6-fluorobenzoxazole-4-carboxylate (0.95 g, 87%). 1H NMR and MS consistent.

1. customthe resulting reaction mixture
2. temperaturewas heated
3. temperatureto reflux for 6 h
4. concentrationconcentrated under reduced pressure
5. dissolutionThe residue was dissolved in EtOAc (200 mL)
6. washwashed with H2O (4×100 mL), saturated aqueous ammonium chloride (2×100 mL), brine (2×100 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure