Sorafenib IMpurity

Uses

Methyl 4-(Methylamino)picolinate is a pyridinyl building block and a useful synthetic intermediate.

Synthesis

Add 0.8 g (0.004 mol) of 2-chloro-3-trifluoromethyl aniline and 0.7 g (0.004 mol) of N,N-carbonyl diimidazole to 10 mL of dichloromethane, stirring at room temperature for 4 h. Add 0.6 g (0.002 mol) of Compound 2, stirring for 6 h. Distil under reduced pressure and purify by column chromatographic separation (silica gel 200-300 mesh; eluent: V (hexane ):V(ethyl acetate)=5:1), concentrated to dryness to obtain 0.5g product 4-{4-[3-(2-chloro-3-trifluoromethyl-phenyl)-acyl urea]-phenoxy}-pyridine-2-carboxylic acid methyl amine, yield 43.5%, m.p. 188190C, purity 96.7%. (HPLC method: octadecylsilane-bonded silica gel as filler, mobile phase A: phosphate buffer, mobile phase B: V (acetonitrile):V (ethanol) = 70:30, flow rate 0.8 mL/min, detection wavelength 240 nm, RT = 29.61 min).