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5-bromo-3-methyl-2-(methylsulfonyl)Pyridine synthesis

2synthesis methods
1289270-74-1 Synthesis
5-Bromo-3-methyl-2-(methylthio)pyridine

1289270-74-1
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5-bromo-3-methyl-2-(methylsulfonyl)Pyridine

1445651-58-0
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Yield:1445651-58-0 96%

Reaction Conditions:

with 3-chloro-benzenecarboperoxoic acid in dichloromethane at 0 - 20;

Steps:

B23.2 5-Bromo-3-methyl-2-(methylsulfonyl)pyridine (B23.2)

5-Bromo-3-methyl-2-(methylsulfonyl)pyridine (B23.2) (0425) To a mixture of B23.1 (1.1 g, 5 mmol) in DCM (11 mL) was added m-CPBA (2.58 g, 15 mmol) at 0° C. The mixture was stirred overnight at rt, then quenched by 2 mol/L aq. NaOH solution (50 mL), extracted with ethyl acetate (50 mL×2). The combined organic layers were washed successively with 50 mL H2O and 50 mL brine, dried over Na2SO4, concentrated to give the title compound (1.2 g, 96%) as a white solid. LC-MS: [M+H]+=249.9.

References:

US2016/176882,2016,A1 Location in patent:Paragraph 0423; 0425