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Production process of evodiamine and method for recycling solvent in production

A production process, the technology of evodiamine, applied in the field of organic synthesis, can solve the problems of high price, high toxicity and difficult operation

Inactive Publication Date: 2021-02-23
ZHANG JIA GANG VINSCE BIO PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, phosgene is useful in 2), 3), which is extremely toxic and difficult to operate in industry
4) Triphenylphosphine and mercuric acetate are used, which is not only expensive, but also pollutes a lot
1), 5) Ethyl chloroformate is used, which is highly toxic and controlled by the public security department, and is not suitable for large-scale industrial production

Method used

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  • Production process of evodiamine and method for recycling solvent in production
  • Production process of evodiamine and method for recycling solvent in production
  • Production process of evodiamine and method for recycling solvent in production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A kind of synthetic method of evodiamine

[0044] Step 1) tryptamine (160g, 1mol) was mixed with ethyl formate (960ml), and refluxed at 70°C for 12 hours. After the reaction, the temperature was lowered to 25°C, and ethyl formate was obtained by distillation under reduced pressure. The solid was washed with dichloromethane ( 500ml) was dissolved, washed with 50ml of water, the dichloromethane phase was dried over anhydrous sodium sulfate, filtered, and concentrated to obtain intermediate product A (172g, 0.91mol) with a purity of 98%. Ethyl formate was reserved for future use.

[0045] Step 2) Dissolve intermediate product A (172.1g, 0.91mol) in ethyl acetate (1.1L), cool down to 5°C, add trichlorophosphoric acid (238.7g, 1.56mol), react for 2 hours, raise to 25°C, After the reaction was complete, water (1.8 L) was added and the pH was adjusted to 10 with saturated potassium carbonate solution, and the aqueous phase was extracted several times with ethyl acetate until ...

Embodiment 2

[0048] Solvent recovery

[0049] S1: multiple batches of ethyl formate obtained in Example 1 were combined, and DMF with 1.8 times the volume of ethyl formate was added to a dividing wall extractive distillation column for rectification;

[0050]S2: Collect the fraction at 53-58°C in the extraction and rectification section of area I to obtain ethyl formate; the fraction at 78-83°C in the side line rectification section of area II is used for waste liquid treatment; the rest is in the public stripping section of area III The liquid of the segment is DMF.

[0051] The purity of ethyl formate detected by HPLC was 99.7%, and the purity of DMF was 99.9%.

[0052] Example 3 - The difference with Example 1 is the use of recovered ethyl formate and DMF

[0053] A kind of synthetic method of evodiamine

[0054] Step 1) tryptamine (160g, 1mol) was mixed with ethyl formate (960ml) recovered in Example 2, and refluxed at 70°C for 12 hours. After the reaction, the temperature was lower...

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Abstract

The invention relates to the field of organic synthesis, in particular to a production process of evodiamine and a method for recycling a solvent in production. According to the method, tryptamine isadopted as a raw material, evodiamine is obtained through formylation, cyclization and condensation ring closing, phosgene and ethyl chloroformate are prevented from being used in the whole process, the safety risk in the production process is reduced, and the reaction steps are greatly simplified. Meanwhile, a solvent application process in production is realized, so that the production cost is greatly reduced, and the method has an industrial popularization value.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a production process of evodiamine and a method for recovering mechanically applied solvents during production. Background technique [0002] Evodia rutaecarpa is the dry and nearly ripe fruit of Ruecarpa rutaecarpa. As a traditional Chinese medicine, it has the functions of strengthening the heart, calming the nerves, antibacterial, reducing blood pressure, analgesia, and improving brain function. It can be used to treat diseases such as high blood pressure, headache, dysmenorrhea, and dysentery. Body system disorders have a good recovery and regulation effect. The research on the main active ingredients of Evodiamine and their pharmacological effects shows that Evodiamine, as one of the main active ingredients of Evodiamine, has analgesic and anti-inflammatory properties, bronchial contraction, and temperature regulation. Weight loss and other effects. In recent years, with th...

Claims

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Application Information

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IPC IPC(8): C07D471/14C07C67/54C07C69/06C07C231/24C07C233/03
CPCC07C67/54C07C231/24C07D471/14C07C69/06C07C233/03
Inventor 彭学东张梅赵金召
Owner ZHANG JIA GANG VINSCE BIO PHARM
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