反应详情

温度

120 °C

The 4-acetyl-6-chloro-3-ethoxy-2-iodobenzonitrile (0.20 g, 0.57 mmol) was combined with pyrrolidine (0.052 mL, 0.63 mmol) in N,N-dimethylformamide (2.0 mL) with cesium carbonate (0.19 g, 0.57 mmol) and heated to 120° C. in a sealed tube. After heating for 18 hrs the reaction was allowed to cool, taken up in ethyl acetate, washed with water, brine, dried over magnesium sulfate and concentrated to give the crude product as a dark oil. The product was purified by FCC on silica gel eluting with hexane:ethyl acetate gradient to give 4-acetyl-6-chloro-3-ethoxy-2-pyrrolidin-1-ylbenzonitrile as an oil (0.045 g, 27%). LCMS calculated for C15H18ClN2O2(M+H)+: m/z=293.1; found 293.1.

1. temperatureAfter heating for 18 hrs the reaction
2. temperatureto cool
3. washwashed with water, brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customto give the crude product as a dark oil
7. customThe product was purified by FCC on silica gel eluting with hexane