反应详情

温度

100 °C

To a solution of 9-(8-aza-bicyclo[3.2.1]oct-3-ylidene)-9H-xanthene-3-carboxylic acid diethylamide, 8a (3 g, 7.7 mmol) in chloroform (50 mL) were added ethanol (2.25 mL, 38.6 mmol) and trimethylsilyl iodide (5.25 mL, 38.6 mmol). The mixture was stirred at 100° C. for 2 h in a sealed tube. The reaction was allowed to cool to rt and washed with 1 N NaOH, aqueous Na2S2O4, and brine. The organic phase was dried over sodium sulfate, filtered, and concentrated, to yield title compound 9-(8-aza-bicyclo[3.2.1]oct-3-yl)-9H-xanthene-3-carboxylic acid diethylamide, 9a (3.0 g, 0.53 mmol). MS m/z=391.4 (MH+)

1. temperatureto cool to rt
2. washwashed with 1 N NaOH, aqueous Na2S2O4, and brine
3. dry with materialThe organic phase was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated