反应详情

温度

100 °C

A mixture of 1-benzyl-3-ethoxycarbonyl-4-piperidone hydrochloride (0.285 g, 0.96 mmol), 2-chloroacetamidine hydrochloride (0.149 g, 1.16 mmol) and sodium methoxide (1.9 ml of a 25% wt/wt solution in methanol) and methanol (0.5 mL) was heated in a sealed tube in microwave (Emrys Optimizer model, Personal Chemistry) at 100° C. for 15 min. The mixture was allowed to cool to r.t. and concentrated under reduced pressure to leave a brown solid. The solid was taken up in water (30 mL) and extracted with a 3:1 mixture of chloroform:isopropanol (3×30 mL). The combined organic extracts were dried over sodium sulfate and concentrated to dryness to leave the title compound (0.196 g, 72%) which was used directly without further purification.

1. temperatureto cool to r.t.
2. concentrationconcentrated under reduced pressure
3. customto leave a brown solid
4. extractionextracted with a 3:1 mixture of chloroform
5. dry with materialThe combined organic extracts were dried over sodium sulfate
6. concentrationconcentrated to dryness