A kind of synthetic method of bispiperidinyl-2-alcohol
A technology of bis-piperidinyl and synthesis method is applied in the field of synthesizing bis-piperidinyl-2-ol, which can solve the problems of few product varieties and limited application coverage, achieve simple and easy reaction operation, and improve anode polarization. performance, effect of inhibiting corrosion
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Embodiment 1
[0018] In a four-neck flask equipped with a stirring device, a reflux condenser and a thermometer, add 129 grams of benzene, 1.1 grams of zinc chloride and 51.6 grams of piperidine, and slowly add 28 grams of chloropropylene oxide under stirring conditions. The reaction was refluxed at 80℃~85℃ for 3 hours to produce the intermediate product monopiperidin-2-ol. A saturated aqueous potassium carbonate solution was added to the reaction mixture, and the temperature was raised to 85℃~90℃ to continue the reflux reaction for 5 hours. During the reaction Use a saturated aqueous solution of potassium carbonate to control the pH at 8-9 to produce bispiperidin-2-ol. After the reaction is completed, cool to 25-35°C, stop stirring, and let stand. The reaction mixture is divided into two layers, the upper layer is the organic phase , Separate the lower layer containing the sediment, add water to dilute and dissolve the sediment, extract the lower diluted solution twice with 51.6 g of benzene...
Embodiment 2
[0020] In a four-neck flask equipped with a stirring device, a reflux condenser and a thermometer, add 120 grams of benzene, add 0.4 grams of zinc chloride, 0.32 grams of zinc hydroxide and 60 grams of piperidine, and slowly add 30 grams of chlorinated Butylene oxide, reflux reaction at 85℃~90℃ for 4 hours to produce the intermediate product monopiperidin-2-ol. Add 20% potassium hydroxide solution to the reaction mixture, and then heat to 90℃~95℃ to continue The reaction was refluxed for 3 hours. During the reaction, the pH was controlled at 8-9 with 20% potassium hydroxide solution to generate bispiperidin-2-ol. After the reaction, it was cooled to 30-40°C, the stirring was stopped, and the reaction was allowed to stand still. The mixture is divided into two layers, the upper layer is the organic phase, the lower layer containing the sediment is separated, the lower layer is diluted and dissolved by adding water, and the lower layer diluted solution is extracted twice with 54 g...
Embodiment 3
[0022] In a four-neck flask equipped with a stirring device, a reflux condenser and a thermometer, add 134 grams of benzene, add 0.30 grams of zinc chloride, 0.22 grams of zinc hydroxide and 89 grams of piperidine, slowly add 32 grams of chlorinated Butylene oxide, reflux reaction at 80℃~90℃ for 3.5 hours to produce the intermediate product monopiperidin-2-ol. Add 20% potassium hydroxide solution to the reaction mixture, and then heat to 85℃~95℃ to continue The reaction was refluxed for 4 hours. During the reaction, the pH was controlled at 8-9 with 20% potassium hydroxide solution to generate bispiperidin-2-ol. After the reaction was completed, cooled to 20-30°C, stopped stirring, stood still, and reacted. The mixture is divided into two layers. The upper layer is the organic phase. The lower layer containing the sediment is separated. The lower layer is diluted and dissolved by adding water. The lower layer diluted solution is extracted twice with 72 grams of benzene. The uppe...
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