反应详情

0.102 g (0.273 mmol) of the above (example 45A]) prepared 2-bromomethyl-6-(4-trifluoromethyl-phenyl)-nicotinic acid methyl ester was dissolved in 1.5 ml of acetonitrile and treated with 0.027 g (0.331 mmol) of dimethylamine hydrochloride and 0.080 ml (2 eq.) of triethylamine. After stirring for 2 h at ambient temperature, the reaction mixture was poured onto crashed ice/KHSO4-solution and extracted twice with AcOEt. Washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, AcOEt/MeOH/NEt3=9/1/0.05), produced 0.047 g of pure title compound as off-white crystals.

1. additionthe reaction mixture was poured
2. extractionextracted twice with AcOEt
3. washWashing with water and brine
4. dry with materialdrying over magnesium sulfate, and evaporation of the solvents