反应详情

温度

40 °C

0.5 g (1.7 mmol) of 4-cyclopentylamino-3-methyl-iodobenzene are dissolved in 20 ml tetrahydrofuran and after the addition of 81.3 mg (1.7 mmol) of sodium hydride (50% in oil) stirred for 1 hour at 40 ° C. After cooling to ambient temperature 0.1 ml (1.5 mmol) of acetyl chloride is added and the mixture is stirred overnight at ambient temperature. The solvent is distilled off and the residue distributed in water/ethyl acetate. The combined organic extracts are dried, concentrated by evaporation and chromatographed on silica gel, eluting with dichloromethane/ethanol 0 to 5%.

1. additionis added
2. stirringthe mixture is stirred overnight at ambient temperature
3. distillationThe solvent is distilled off
4. customThe combined organic extracts are dried
5. concentrationconcentrated by evaporation
6. customchromatographed on silica gel
7. washeluting with dichloromethane/ethanol 0 to 5%