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With tert.-butylnitrite; copper dichloride; In dichloromethane; at 20℃; for 0.5h;
Intermediate IXc 3 ,6-dichloro-2-methylpyridine To a suspension of <strong>[36936-23-9]5-chloro-6-methylpyridin-2-amine</strong> (7.5 g, 52.60 mmol, Combi- Blocks) in DCM (200 niL) was added copper(II) chloride (9.19 g, 68.38 mmol) and stirred at for 10 min. tert-butyl nitrite (12.50 mL, 105.20 mmol) was added and the stirring was continued further 30 min at RT. The colour was changed to dark blue. The reaction was monitored by LCMS. LCMS showed the completion of reaction. The reaction mixture was washed with water, brine solution, and organic layer was dried on sodium sulphate and concentrated under vacuum to get crude. The product was purified by column chromatography using 5 % ethyl acetate :hexane mixture to get 3,6-dichloro- 2-methylpyridine (3.80 g, 44.6 %) as a yellow liquid. MS (ES+), (M+H)+ = 162.15 for C6H5C12N.
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