1-Boc-3-piperidone, is used as an important raw material and intermediate used in organic Synthesis, pharmaceuticals, agrochemicals and dyestuff.
With 179g compound 3(1-BOC-3-piperidines alcohol) drop in the 2L reaction flask, drop into pimelinketone 1300g, aluminum isopropylate 88g, methylene dichloride 400ml is warming up to 80 ℃, insulation reaction 8h, reaction finishes to be cooled to room temperature, adds 10% sodium hydroxide 200ml, stirring at normal temperature 30min, filter, the filtrate normal pressure reclaims methylene dichloride, reclaim under reduced pressure pimelinketone again, reclaim finish after, add the 300ml dichloromethane extraction three times, it is dry concentrated to merge oil reservoir, gets 1-BOC-3-piperidone crude product.
Refining: with 1-BOC-3-piperidone crude product is that 60pa, temperature are to distill under 104 ~ 105 ℃ the condition at pressure, gets 1-BOC-3-piperidone elaboration 163g, 92.9%.