preparation | under the protection of high purity nitrogen, 0.05mmol heteronuclear ruthenium palladium bicyclic metal compound 1, 1mmol o-iodoacetophenone, 2.5mmol benzyl alcohol, 2mmol potassium hydroxide and 3ml dioxane are added to 10ml of Schlek reaction tube, and the reaction tube is replaced three times with nitrogen, then it is heated to 110 ℃ in an oil bath under magnetic stirring, and the reaction is refluxed for 30 hours. Remove the oil bath and reduce the water bath to room temperature; Add 3ml of water to the reaction liquid, extract it three times with 5ml of dichloromethane, combine the organic phase and dry it with anhydrous MgSO4 for 30 minutes, filter, concentrate the filtrate with a rotary evaporator, and use the dichloromethane/petroleum ether mixture as the developing agent to separate it with silica gel thin layer chromatography to obtain the pure product 3-phenyl-1-indanone. |