反应详情

To a mixture of triphenylmethylphosphonium iodide (22.14 g) in toluene (135 ml) was added potassium tert-butanolate (5.32 g). The solution turned to orange. Then N-Boc-3-piperidone (6.0 g) in toluene (66 ml) was dropped into the solution under argon, at 30° C. The reaction was filtered and washed with water (200 ml, 2×) and then diluted by HCl (1M), dried with anhydrous sodium sulfate. The solution was purified by flash chromatography (silica gel, PE:EA=15:1) to obtain N-Boc-3-methylenepiperidine as an oil (4.2 g).

1. filtrationThe reaction was filtered
2. washwashed with water (200 ml, 2×)
3. additiondiluted by HCl (1M)
4. dry with materialdried with anhydrous sodium sulfate
5. customThe solution was purified by flash chromatography (silica gel, PE:EA=15:1)