5-Bromo-3-methyl-2-(methylthio)pyridine synthesis

Yield:1289270-74-1 95%

Reaction Conditions:

in N,N-dimethyl-formamide at 0; for 3.5 h;Inert atmosphere;

Steps:

B23.1 5-Bromo-3-methyl-2-(methylthio)pyridine (B23.1)

5-Bromo-3-methyl-2-(methylthio)pyridine (B23.1) (0424) A mixture of 5-bromo-2-fluoro-3-methylpyridine (1 g, 5.26 mmol), CH₃SNa (479 mg, 6.84 mmol) in DMF (10 mL) was stirred for 3.5 h at 0° C. under N₂. The mixture was diluted with 50 mL water, extracted with ethyl acetate (50 mL×3). The combined organic layers were successively washed with 50 mL water and 50 mL brine, dried over Na₂SO₄, concentrated to give the title compound (1.1 g, 95%) as a white solid. LC-MS: [M+H]⁺=218.

References:

US2016/176882,2016,A1 Location in patent:Paragraph 0423; 0424