1-Benzyl-3-piperidone synthesis

10synthesis methods

Product Name:1-Benzyl-3-piperidone
CAS Number:40114-49-6
Molecular formula:C12H15NO
Molecular Weight:189.25

4-(BENZYL-ETHOXYCARBONYLMETHYL-AMINO)-BUTYRIC ACID ETHYL ESTER

63876-32-4
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40114-49-6
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$90.00/10g

Yield:40114-49-6 86.9%

Reaction Conditions:

with potassium tert-butylate in tetrahydrofuran at 50 - 60; for 3 h;

Steps:

4 Example 4: Preparation of N-benzylpiperidin-3-one
Stirring,thermometer,In a 500 ml four-necked flask with a reflux condenser and a dropping funnel,Add 200 g of tetrahydrofuran, 15.0 g (0.13 mol) of potassium t-butoxide,A mixture of 30.7 g (0.1 mol) of N-benzyl-3-aza-1,7-pimelic acid diethyl ester and 50 g of tetrahydrofuran was added dropwise between 50 and 55 ° C, and the mixture was stirred at 55 to 60 ° C. 3 hours.Cool to 30 to 35 ° C, add 100 grams of water, and stir the reaction at 30 to 35 ° C for 2 hours.The pH of the acidification system was adjusted to 2.0-2.5 with 30% hydrochloric acid, and the reaction was stirred at 30 to 35 ° C for 0.5 hour.Add 100 g of dichloromethane, separate the layers, and extract the aqueous layer with dichloromethane for 3 times, 30 g each time.The organic phases were combined, and dichloromethane was distilled to give 16.4 g of N-benzylpiperidin-3-one.The yield was 86.9%, and the liquid phase purity was 99.6%

References:

Xin Fa Pharmaceutical Co., Ltd.;Qi Yuxin;Ju Lizhu;Zhang Mingfeng;Lv Qiangsan;Wang Tao CN110240561, 2019, A Location in patent:Paragraph 0057-0058; 0073; 0074

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