1721-23-9

58539-65-4

177662-40-7

1721-23-9

Step 2 Preparation of 3-cyano-2-methylpyridine: Trifluoroacetic anhydride (21.0 g, 0.100 mol) was rapidly added to a 400 mL dichloromethane suspension containing 2-methylnicotinamide (11.1 g, 0.081 mol) and triethylamine (24.8 g, 0.243 mol) at 0 °C. The reaction was carried out at 0 °C for a few minutes and completed. Subsequently, water was added and the aqueous layer was extracted with dichloromethane. The combined organic layers were washed sequentially with water and brine and dried with anhydrous magnesium sulfate. After filtration, the filtrate was concentrated and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane, 1:1) to give 7.2 g of 3-cyano-2-methylpyridine as a light yellow solid in 75% yield. Melting point (DSC) 56°-58°C.