Pipecolinic acid preparation process based on reverse dropping

A preparation process, pipecolic acid technology, applied in the field of medicine, can solve the problems of long time, long preparation time, and difficult difficulty reduction, and achieve the effect of improving preparation efficiency, reducing duration, and good mixing effect

Inactive Publication Date: 2019-09-10
BTC PHARMA TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The pipecolic acid prepared by the present invention is specifically 3-[(1,1-dimethylethyl) dimethylsiloxo]-2-aminopropyl-dimethylethyl ester-1-pipercolic acid, But because the preparation process of 3-[(1,1-dimethylethyl) dimethylsiloxo]-2-aminopropyl-dimethylethyl ester-1-pipericolic acid is extremely complicated, and its The required preparation time is extremely long, and in the entire preparation process

Method used

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  • Pipecolinic acid preparation process based on reverse dropping
  • Pipecolinic acid preparation process based on reverse dropping
  • Pipecolinic acid preparation process based on reverse dropping

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Embodiment 1

[0062] see Figure 1-15 , a pipecolic acid preparation process based on reverse dropwise addition, comprising the following steps:

[0063] S1, 6Kg raw material 1, 4.7Kg triethylamine, 50g DMAP were dissolved in 36Kg dichloromethane, cooled to 0-20°C, 3.2Kg pivaloyl chloride was added dropwise, the temperature was controlled at 0-5°C, and the addition was completed in 10 hours, 0- Stir and react at 5°C for 1 hour, GC detection of pivaloyl chloride ≤ 1%; directly add 40Kg of water to quench, stir and separate the liquid, then wash with 30Kg of 5% citric acid aqueous solution to weak acidity, dry the organic phase with anhydrous sodium sulfate, and filter , the solution is waiting for the next step;

[0064] S2. Add 2, sodium acetate, Tempo, anhydrous sodium sulfate and DCM to a 50L reactor, and react at a temperature of 10-20°C for 5 hours; GC detection shows that the content of 2 is less than or equal to 5%, and the material is discharged and filtered, 10Kg 5% sulfur Wash wi...

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Abstract

The invention discloses a pipecolinic acid preparation process based on reverse dropping and belongs to the technical field of medicines. By adopting the pipecolinic acid preparation process based onreverse dropping, S1-S2 and S3-S7 can be implemented simultaneously, so that the lasting time of the whole preparation process can be effectively shortened; meanwhile, by adopting a dropping mode in the preparation process, a conventional mode of dropping from top to bottom is changed into a mode of dropping from bottom to top, small water domes can be formed because of instantaneous impact resulted when a liquid to be dropped is fed into a reaction kettle, and are diffused outwards and upwards, liquid convection of the dropped liquid and a reactant can be enhanced because of the water domes,thus a good mixing effect is achieved, reactions can be accelerated to a certain extent, the preparation efficiency can be improved, and compared with the mode of dropping from top to bottom, the process is capable of effectively avoiding the phenomenon that the content of the reactant is changed to a certain extent as the liquid is splashed because of water impact and is adhered to an inner wall.

Description

technical field [0001] The invention relates to the technical field of medicine, and more specifically, relates to a pipecolic acid preparation process based on reverse dropwise addition. Background technique [0002] Pipecolic acid (PA) is an important rigid cyclic non-protein amino acid, which can not only limit the conformation of polypeptides, but also serve as a multifunctional backbone in the synthesis library of different compounds, so it is widely used in many chiral Preparation of pharmaceuticals and biologically active substances. For example, the new-generation local anesthetic Ropivacaine, the antipsychotic drug Thioridazine, the immunosuppressant Rapamycin, and the antitumor antibiotic Sandramycin are all based on Pipecolic acid or its derivatives are the main raw materials. [0003] Due to the biological activity and wide application prospects of pipecolic acid and its derivatives, its synthesis has attracted the interest of many foreign researchers, and many...

Claims

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Application Information

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IPC IPC(8): C07D211/42
CPCC07D211/42
Inventor 陈国庆杨少强曹众李怀鑫张灵龙陆毅周广徐本全吴林艳
Owner BTC PHARMA TECH CO LTD
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