反应详情

To a solution of 1-(5-Bromo-pyridin-2-yl)-2,2,2-trifluoro-ethanone (7.5 g, 29.52 mmol) in dry toluene (30 mL) is added benzylamine (3.15 g, 29.52 mmol) and titanium ethoxide (7.4 g, 32.48 mmol) at room temperature then stir for 3 hours. Reaction mixture is diluted with saturated sodium bicarbonate solution and extracted with ethyl acetate. Organic layer is dried over sodium sulphate, solvent is evaporated in vacuo and purified by column chromatography eluting in 20% ethyl acetate in hexane to afford the title compound (0.45 g). LC-MS (m/z): [M+H]=345.0.

1. customReaction mixture
2. extractionextracted with ethyl acetate
3. dry with materialOrganic layer is dried over sodium sulphate, solvent
4. customis evaporated in vacuo
5. custompurified by column chromatography
6. washeluting in 20% ethyl acetate in hexane