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To a solution of <strong>[3430-29-3]3,5-dibromo-4-methyl-pyridin-2-ylamine</strong> (3.38 g, 12.7 mmol) in THF (60 mL) cooled to -78 C. was added n-BuLi (1.9M in pentane) (13.4 mL, 25.4 mmol) to give an orange solution. The solution was stirred at -78 C. for 1 h and then quenched with water (10 mL). The pH of the mixture was adjusted to ~12 with 10N NaOH and then extracted with CH2Cl2 (3*30 mL), dried (Na2SO4), filtered and concentrated in vacuo to give an orange oil. Purification by column chromatography on silica gel (Et2O) afforded 3-bromo-4-methyl-pyridin-2-ylamine (1.68 g, 71%) as a pale yellow solid. 1H NMR (CDCl3) delta 2.32 (s, 3H), 5.00 (br s, 2H), 6.52 (d, 1H, J=6.0 Hz), 7.84 (d, 1H, J=6.0 Hz).
1 g
With n-butyllithium; In tetrahydrofuran; hexane; at -78℃; for 1h;
To a THF solution (40.0 mL) of <strong>[3430-29-3]2-amino-3,5-dibromo-4-methylpyridine</strong> (2.00 g) was added n-butyllithium (1.67 mol/L hexane solution, 9.0 mL) at -78C, and the reaction mixture was stirred at the same temperature for 1 h Water was added, and the mixture was extracted twice with chloroform. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated, and the obtained residue was purified by silica gel column chromatography (solvent; hexane/ethyl acetate=85/15 - 60/40) to give the title compound (1.00 g). MS(ESI)m/z; 187,189[M+H]+
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