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Method for removing by-product dimethyl sulfide in moxidectin production process

A technology for the production process of dimethyl sulfide, applied in the field of eliminating the by-product dimethyl sulfide in the production process of moxictine, can solve the problems of low boiling point, nasal irritation, flammability, etc., and achieve the absorption process Simple, optimized production environment, low cost of raw materials

Inactive Publication Date: 2015-01-21
大连九港生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the above-mentioned process of producing moxictine, the oxidation step uses "activated dimethyl sulfoxide reagent" (see: Synthesis, 1990, 857-870; Synthesis, 1981, 165-185;) as the oxidation system in many process routes , For example, systems such as dimethyl sulfoxide / phenyl dichlorophosphate, dimethyl sulfoxide / pyridine sulfur trioxide, dimethyl sulfoxide / phosphorus pentoxide (see: US4988824, 1991; CN1051043, 1991), These systems are non-metal oxidation systems, which avoid the shortcoming of metal residues polluting the final product, but the by-product dimethyl sulfide produced during the oxidation process has the characteristics of low boiling point, volatile, flammable, foul smell, and irritating to the nose. (See: Commonly Used Chemical Dangerous Goods Safety Handbook, Volume One, First Edition, China Medical Science and Technology Press, 1992), which seriously affects the production and operation environment of oxidation and subsequent steps

Method used

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  • Method for removing by-product dimethyl sulfide in moxidectin production process
  • Method for removing by-product dimethyl sulfide in moxidectin production process
  • Method for removing by-product dimethyl sulfide in moxidectin production process

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Effect test

Embodiment 1

[0027] Dissolving nimoctine in the reaction solvent methylene chloride, then adding the acid-binding agent triethylamine and the upper protection reagent 4-chlorophenoxyacetyl chloride, fully stirring until the end of the reaction, adding excess water to quench the reaction solution, Separate the oil layer, obtain the nimoctine with protective group through drying and precipitating, combine it with activated dimethyl sulfoxide reagent (dimethyl sulfoxide / phenyl dichlorophosphate), acid-binding agent triethylamine and the solvent dichloromethane used in the oxidation step are mixed for oxidation reaction. After reaching the end point of the reaction, an excessive amount of water is added to quench the oxidation reaction solution, and then a nitrogen blowing precipitation device is connected, and the nitrogen flow rate is controlled at 30mL / min. Control at 25-30°C, and control the temperature of the absorption tank and condenser with 50g of sodium hypochlorite solution (5 times t...

Embodiment 2

[0029] Dissolving nimoctine in the reaction solvent methylene chloride, then adding the acid-binding agent triethylamine and the upper protection reagent 4-chlorophenoxyacetyl chloride, fully stirring until the end of the reaction, adding excess water to quench the reaction solution, Separate the oil layer, obtain the nimoctine with protective group through drying and precipitating, combine it with activated dimethyl sulfoxide reagent (dimethyl sulfoxide / phenyl dichlorophosphate), acid-binding agent triethylamine And the solvent dichloromethane used in the oxidation step is mixed to carry out the oxidation reaction. After reaching the end of the reaction, add excess water to quench the oxidation reaction solution, and then connect to the nitrogen blowing precipitation device. The nitrogen flow rate is controlled at 300mL / min. Control at 18-22°C, and control the temperature of the absorption kettle and condenser with 150g of sodium hypochlorite solution (7 times the amount of th...

Embodiment 3

[0031]Dissolving nimoctine in the reaction solvent methylene chloride, then adding the acid-binding agent triethylamine and the upper protection reagent 4-chlorophenoxyacetyl chloride, fully stirring until the end of the reaction, adding excess water to quench the reaction solution, Separate the oil layer, obtain the nimoctine with protective group through drying and precipitating, combine it with activated dimethyl sulfoxide reagent (dimethyl sulfoxide / phenyl dichlorophosphate), acid-binding agent triethylamine and the solvent methylene chloride used in the oxidation step are mixed for oxidation reaction. After reaching the end of the reaction, excess water is added to quench the oxidation reaction solution, and then connected to a negative pressure precipitation device. The temperature of the oxidation reaction kettle is controlled at 25-30 ° C. The temperature of the absorption kettle and condenser with 100g of sodium hypochlorite solution is controlled at 0-5°C, and then he...

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Abstract

The invention discloses a method for removing by-product dimethyl sulfide in a moxidectin production process, and belongs to the technical field of chemical industry production. The method comprises the following steps: in the production process of moxidectin, after oxidation reaction steps are ended, adding excessive water quenching reaction liquid to oxidation reaction liquid; transferring a by-product dimethyl sulfide generated in the oxidation step and used solvent to a sodium hypochlorite absorption kettle through a condenser in a manner of advocating gas desolvation or negative pressure desolvation; oxidizing and absorbing dimethyl sulfide through a sodium hypochlorite solution in the sodium hypochlorite absorption kettle and recovering a reaction solvent, wherein the content of dimethyl sulfide contained in oxidation reaction can be quickly reduced to 1.0% or less, the solvent recovery rate is greater than 60%, and the method has the advantages of low raw material cost, simple absorption process and the like.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a method for eliminating dimethyl sulfide, a by-product in the production process of moxictine. Background technique [0002] Moxictine is a semi-synthetic macrolide drug with good anthelmintic activity, long-acting and safe properties. Cyclic lactone anthelmintic antibiotics (see: Parasites & Vectors2009, 2(Suppl2), S5). At present, the main way to produce moxictine is to use nimoctine as a raw material, which is obtained through four chemical reaction steps of upprotection, oxidation, oximation and deprotection (see: Chinese patent application 201410272172; AU2006203459, 2006; US4988824 , 1991), the specific chemical reaction process see figure 1 . [0003] In the above-mentioned process of producing moxictine, the oxidation step uses "activated dimethyl sulfoxide reagent" (see: Synthesis, 1990, 857-870; Synthesis, 1981, 165-185;) as the oxidation system in many ...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 戴耀李贺先王荣良
Owner 大连九港生物科技有限公司
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