Analyzing the synthesis route of 72752-52-4

72752-52-4 2-Piperidinobenzonitrile 2774355, apiperidines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.72752-52-4,2-Piperidinobenzonitrile,as a common compound, the synthetic route is as follows.

72752-52-4, A mixture of iBuMgBr (2 M in diethyl ether, 1.6 l, 3.2 mol) and toluene (1.6 1) was heated to a temperature of about 87C under nitrogen atmosphere. Then a solution of 2-piperidino-benzonitril (300 g, 1.6 mol) in toluene (1.6 1) was slowly added to the hot mixture within 1h, while maintaining the temperature. Thereafter, the reaction mixture was heated to reflux at a temperature of about 103-105C for 3h. After cooling the mixture to 0C, 1.6 1 of methanol were slowly added to this mixture. The resulting mixture was stirred for another hour at about 0-5C. Then NaBH4 (121 g, 3.2 mol) was added successively within 1h. Thereafter, the mixture was stirred for another hour at 15C and for another 2 hours at room temperature. Then 1.6 1 of THF was added and the mixture was stirred over night. The precipitated salts were filtrated and washed with THF (2 x 400 ml) and water (2 x 1.6 1) twice. The filtrate was dried and evaporated in vacuo to give 352 g of a crude yellow oil, which was then dissolved in 2-propanole (3.2 1). This solution was heated to a temperature of about 50C, at which 180 g of glutaric acid was slowly added. The product precipitated from this solution was stirred for 2h at room temperature and for 2h at 0-5C. After filtration and washing with cold 2-propanole (300 ml), the wet product was dried in a vacuum drier at 60C for 18h, to give 463 g (76%) of the desired product.

72752-52-4 2-Piperidinobenzonitrile 2774355, apiperidines compound, is more and more widely used in various fields.

Reference:
Patent; Krka Tovarna Zdravil, D.D., Novo Mesto; EP2177221; (2010); A1;,
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