反应详情

30.0 g (0.15 mol) of 4-bromomethyl-benzonitrile, 2.0 ml (0.12 mol) of iron pentacarbonyl, 29.0 g potassium carbonate, 10.0 ml mesitylene and 250 ml absolute methanol are placed in a pressure vessel and about 3.5 l carbon monoxide gas is introduced. The reaction mixture is shaken for 16 hours at ambient temperature, mixed with water, neutralised with hydrochloric acid and extracted with ethyl acetate. The combined organic extracts are washed with sodium hydrogen carbonate solution, dried and evaporated down. The residue is chromatographed on silica gel and eluted with petroleum ether/ethyl acetate (9:1, 8:2 and 7:3). The desired fractions are combined and evaporated down.

1. extractionextracted with ethyl acetate
2. washThe combined organic extracts are washed with sodium hydrogen carbonate solution
3. customdried
4. customevaporated down
5. customThe residue is chromatographed on silica gel
6. washeluted with petroleum ether/ethyl acetate (9:1, 8:2 and 7:3)
7. customevaporated down