Hydrochloric Acid → 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile

関与物質

反応手順

101.5 g of 5-Cyano-5-(4-fluoro-phenyl)-2-oxo-cyclohexanecarboxylic acid methyl ester (11) were dissolved in 680 mL of ethanol and 171 mL of concentrated aqueous hydrochloric acid were added. The mixture was heated to reflux for 40 h, then evaporated. The residue was taken up in water and extracted with dichloromethane. The organic layer was washed with brine, dried over magnesium sulphate and evaporated to give 95.2 g of crude product, that was purified by silica gel filtration (heptanes:ethyl acetate) to yield 50.4 g of the desired product 12. Rt=1.26 min (Method 1). Detected mass: 218.2 (M+H+).

情報源と証拠