Synthetic method of emamectin benzoate

A synthetic method and emamectin benzoate technology, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., to achieve the effects of accurate feeding, stable continuous automation, and less material volume

Pending Publication Date: 2022-03-15
QILU SYNVA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention provides a synthetic method of emamectin benzoate in order to solve the problem that the whole process cannot realize stable continuous flow production in the prior art

Method used

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  • Synthetic method of emamectin benzoate
  • Synthetic method of emamectin benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] A kind of synthetic method of emamectin benzoate, comprises the following steps:

[0069] (1) Mix avermectin B1 and dichloromethane in a mass ratio of 1:3 and add them to the dissolving kettle, fully stir and dissolve and lower the temperature to -30°C to obtain the abamectin solution, which is transferred to the abamectin solution Vermectin solution storage tank (1) is stand-by.

[0070] Control the reaction temperature in the protection tank (A / B / C / D) to be -30±5°C. The Abamectin solution prepared in the step (1) enters the A still according to the flow rate of 520Kg / h, and simultaneously pumps allyl chloroformate (protective agent) and tetramethylethylenediamine (alkali) into the A still, The flow rates of the two are controlled at 5.85Kg / h and 10.38Kg / h respectively. After the three materials are fully mixed and reacted in the A tank; the feed liquid enters the B tank through self-flow, and at the same time pumps allyl chloroformate, the flow rate is controlled at...

Embodiment 2

[0083] A kind of synthetic method of emamectin benzoate, comprises the following steps:

[0084] The difference from Example 1 is that,

[0085] Protection process: the protective agent is ethyl chloroformate, the organic base is triethylamine, the molar ratio of abamectin and triethylamine is 1:0.8, and the molar ratio of avermectin and ethyl chloroformate is 1:1.2 , the reaction temperature is -20±5°C.

[0086] Oxidation process: the organic base is triethylamine, and the molar ratio of dimethyl sulfoxide and organic base is 1:1.2.

[0087] Amination process: the temperature is between 40±5°C, acetic acid is replaced by benzoic acid solution, the concentration of benzoic acid solution is 20%, and the molar ratio of compound (formula IV) to benzoic acid is 1:1.2.

[0088] The emamectin benzoate product can be obtained at 147.82kg / h, with a content of 78.1%, a mass yield of 88.8%, and a purity of 85.2%.

Embodiment 3

[0090] A kind of synthetic method of emamectin benzoate, comprises the following steps:

[0091] The difference from Example 1 is that,

[0092] Protection process: the organic base is triethylamine, and the molar ratio of avermectin and triethylamine is 1:0.8.

[0093] Oxidation process: the organic base is triethylamine, the molar ratio of dimethyl sulfoxide and organic base is 1:1.2, the activator is the dichloromethane solution of triphosgene, the concentration of triphosgene is 30%, the compound (formula III) and The molar ratio of triphosgene is 1:0.35, and the reaction temperature is 0±5°C.

[0094] Amination process: temperature is between 40±5°C, acetic acid is replaced by p-toluenesulfonic acid solution, the concentration of p-toluenesulfonic acid solution is 20%, compound (formula IV) and p-toluenesulfonic acid The molar ratio is 1:0.5, and the molar ratio of p-toluenesulfonic acid and methylamine is 1:4.5.

[0095] Deprotection process: the temperature is contro...

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Abstract

The invention discloses a synthetic method of emamectin benzoate. The synthetic method is a continuous preparation method comprising a protection process, an oxidation process, an amination process, a deprotection process and a salification process. The method comprises the following steps: in a protection process, dissolving abamectin (formula II) in alkyl halide to obtain an abamectin solution, and continuously pumping the abamectin solution, alkali and a protective agent into a multi-kettle series device respectively to obtain a mixed reaction solution A containing 5-hydroxyl protected abamectin (formula III); in the deprotection process, inorganic bases such as sodium hydroxide and potassium hydroxide are added into a sodium borohydride alcoholic solution; desalting and filtering are carried out before the amination process. The problem that stable continuous flow production cannot be achieved in the whole process in the emamectin benzoate production process in the prior art is solved, the material amount of online reaction is small, and intrinsic safety can be achieved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthetic method of emamectin benzoate. [0002] technical background [0003] Emamectin benzoate (full name: emamectin benzoate), white or light yellow crystalline powder, soluble in acetone and methanol, slightly soluble in water, insoluble in hexane. Emamectin benzoate is a new type of high-efficiency semi-synthetic antibiotic insecticide, which has the characteristics of ultra-high efficiency, low toxicity (preparation is almost non-toxic), low residue, and pollution-free biological pesticides. It is widely used in the control of various pests on vegetables, fruit trees, cotton and other crops. Emamectin emamectin is synthesized from the fermented product avermectin B1. Natural avermectin contains 8 components, mainly 4 kinds namely A 1a 、A 2a , B 1a and B 2a , its total content ≥ 80%; the corresponding 4 smaller homologues are A 1b 、A 2b , B 1b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H17/08C07C63/08C07C51/41
CPCC07H1/00C07H17/08C07C63/08C07C51/412Y02P20/55
Inventor 薛树会任建海钟行利周士珂罗俊峰刘文耀于晓军徐亚会
Owner QILU SYNVA PHARMA
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