反应详情

温度

0 °C

Under protective gas, 1.6 g (0.053 mol) of sodium hydride (80% strength) are suspended in 50 ml of DMF, 10 g (0.053 mol) of 2-butyl-5-formyl-4-chloroimidazole (preparation according to EP 324,377) in 100 ml of DMF are added dropwise at 0° C., then the mixture is stirred at 0° C. for 15 min and 18.9 g (0.053 mol) of tertbutyl 2-(4-bromomethylphenyl)-2-cyclopentylacetate in 100 ml of DMF are added dropwise. The mixture is stirred for 2 h at 0° C., the solvent is evaporated, the residue is taken up in diethyl ether, the solid is filtered off and, after concentration, the residue is chromatographed on silica gel 60 using dichloromethane. Yield: 16.2 g (66.7% of theory) Solidification point: 101°-102° C.

1. stirringThe mixture is stirred for 2 h at 0° C.
2. customthe solvent is evaporated
3. filtrationthe solid is filtered off
4. concentrationafter concentration
5. customthe residue is chromatographed on silica gel 60 using dichloromethane
6. custom101°-102° C.