反应详情

A 0° C. solution of 2-amino-6-ethylpyridine (3.00 g, 24.56 mmol) in CHCl3 (25 mL) was treated portion-wise with NBS (4.37 g, 24.56 mmol) over 30 minutes, stirred for 45 minutes, then concentrated to dryness. The residue was treated with EtOAc, the solids removed via filtration and the filtrate concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford 5-bromo-6-ethylpyridin-2-amine (3.83 g, 78%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 7.42 (d, J=8.6 Hz, 1H), 6.20 (d, J=8.7 Hz, 1H), 6.03 (s, 2H), 2.60 (q, J=7.5 Hz, 2H), 1.10 (t, J=7.5 Hz, 3H); MS (ESI) m/z: 203.0 (M+H+).

1. concentrationconcentrated to dryness
2. additionThe residue was treated with EtOAc
3. customthe solids removed via filtration
4. concentrationthe filtrate concentrated to dryness
5. custompurified via silica gel chromatography (EtOAc/Hex)