反应详情

4-amino-6-chloro-pyrimidine-5-carbaldehyde Compound 1a (1.0 g), O-methyl-hydroxylamine hydrochloride (0.94 g) and a mixed solvent of acetic acid (25 mL) and H2O (4 mL) were added to a flask. The mixture was stirred at rt overnight, then concentrated. The residue was suspended in H2O and extracted with EtOAc. The organic layer was separated, dried with MgSO4, then concentrated to afford 4-amino-6-chloro-pyrimidine-5-carbaldehyde O-methyl-oxime Compound 9a (0.97 g, 92%). 1H NMR (300 MHz, DMSO-d6) δ 8.55 (s, 1H), 8.50 (s, 1H), 8.25 (s, 1H), 7.70 (s, 1H), 3.98 (s, 3H). MS (ESI) m/z: 188 (M+H+).

1. concentrationconcentrated
2. extractionextracted with EtOAc
3. customThe organic layer was separated
4. dry with materialdried with MgSO4
5. concentrationconcentrated