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Process for continuously synthesizing prochloraz and intermediate acylate of prochloraz active compound

A technology of prochloraz and chemical synthesis, which is applied in the field of continuous synthesis of prochloraz and its technical intermediate acylate, can solve the problems of inconvenient display screen cleaning, circuit damage, poor stability, etc., and achieves shortening the amination reaction time, Cost saving and purity improvement effect

Pending Publication Date: 2021-10-29
江西汇和化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on this, the object of the present invention is to provide a process for the continuous synthesis of prochloraz and its intermediate acylate of the original drug, so as to solve the problems of rainwater easily entering and causing line damage, inconvenient cleaning of the display screen and stability when placed on uneven ground. Poor technical issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A continuous synthesis of prochloraz, comprising the following raw materials by weight: 100 parts of 2,4,6-trichlorophenol, 70-90 parts of liquid caustic soda, 150-190 parts of dichloroethane, 2-5 parts of imidazole, 120-180 parts of propylamine, 25-50 parts of flake alkali, 3-5 parts of antioxidant, 2-3 parts of catalyst, 3-5 parts of stabilizer, 200-250 parts of toluene, 35-45 parts of triethylamine, extraction agent 180-230 parts and trichloromethyl carbonate 120-150 parts.

[0019] A process for continuous synthesis of prochloraz former drug intermediate acylate, its concrete steps are as follows:

[0020] Step 1: Fully dissolve 2,4,6-trichlorophenol and liquid alkali with a concentration of 30%, put in excess dichloroethane, seal and heat up, turn on stirring to fully react, react for 3-5h, and sample and analyze; After passing the test, cool down to 55°C, stop stirring, let stand for stratification for 1 hour, filter out the lower layer water, transfer the materi...

Embodiment 2

[0028] A kind of continuous synthesis of prochloraz, comprising the following raw materials by weight: 100 parts of 2,4,6-trichlorophenol, 90 parts of liquid caustic soda, 190 parts of dichloroethane, 5 parts of imidazole, 1180 parts of propylamine, caustic soda 50 parts, 5 parts of antioxidant, 3 parts of catalyst, 5 parts of stabilizer, 250 parts of toluene, 45 parts of triethylamine, 230 parts of extractant and 150 parts of trichloromethyl carbonate.

[0029] A process for continuous synthesis of prochloraz former drug intermediate acylate, its concrete steps are as follows:

[0030] Step 1: Fully dissolve 2,4,6-trichlorophenol and liquid caustic soda with a concentration of 30%, put in excess dichloroethane, seal and heat up, turn on stirring for full reaction, react for 5h, and sample and analyze; , cooled to 55°C, stopped stirring, left to stand for stratification for 1h, filtered off the lower layer of water, transferred the material to a distillation kettle to remove t...

Embodiment 3

[0038] A continuous synthesis of prochloraz, comprising the following raw materials by weight: 100 parts of 2,4,6-trichlorophenol, 70 parts of liquid caustic soda, 150 parts of dichloroethane, 2 parts of imidazole, 120 parts of propylamine, caustic soda 25 parts, 3 parts of antioxidant, 2 parts of catalyst, 3 parts of stabilizer, 200 parts of toluene, 35 parts of triethylamine, 180 parts of extractant and 120 parts of trichloromethyl carbonate.

[0039] A process for continuous synthesis of prochloraz former drug intermediate acylate, its concrete steps are as follows:

[0040] Step 1: Fully dissolve 2,4,6-trichlorophenol and liquid caustic soda with a concentration of 30%, put in excess dichloroethane, seal and heat up, turn on stirring to fully react, react for 3 hours, and sample and analyze; , cooled to 55°C, stopped stirring, left to stand for stratification for 1h, filtered off the lower layer of water, transferred the material to a distillation kettle to remove the solv...

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Abstract

The invention discloses a process for continuously synthesizing prochloraz and an intermediate acylate of a prochloraz active compound, and relates to the technical field of pesticide chemical engineering. The prochloraz comprises the following raw materials in parts by weight: 100 parts of 2,4, 6-trichlorophenol, 70-90 parts of liquid alkali, 150-190 parts of dichloroethane, 2-5 parts of imidazole, 120-180 parts of propylamine, 25-50 parts of caustic soda flakes, 3-5 parts of an antioxidant, 2-3 parts of a catalyst, 3-5 parts of a stabilizer, 200-250 parts of toluene, 35-45 parts of triethylamine, 180-230 parts of an extraction agent and 120-150 parts of trichloromethyl carbonate. The amination reaction time is shortened, the amination reaction yield is improved, the reaction time is substantially shortened; the conversion rate of the raw materials reaches 98% or above, the yield of the product reaches up to 96%, the purity of the product is improved; the catalyst can be repeatedly used after being soaked in ethanol, the cost is saved; and the process is safe and environment-friendly, is greatly superior to the preparation process in the prior art and is very suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of pesticide chemical industry, in particular to a process for continuously synthesizing prochloraz and its original drug intermediate acylate. Background technique [0002] Prochloraz (Prochloraz), also known as Shi Baoke, Shi Baogong, etc., the chemical name is N-propyl-N-[2-(2,4,6-trichlorophenoxy)ethyl]imidazole-1-methyl Amide is a new type of imidazole broad-spectrum multi-purpose fungicide. [0003] The existing level of prochloraz is relatively backward, and there are often problems such as unsatisfactory efficacy, stratification of preparations, decomposition of the original drug, product precipitation and agglomeration, etc., which greatly limit the development of this dosage form. The production process of prochloraz is complicated, the reaction time is long, the conversion rate is low, and the purity is not high. SUMMARY OF THE INVENTION [0004] Based on this, the object of the present invent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/56B01J23/44
CPCC07D233/56B01J23/44
Inventor 尹旺华韩井卫曾小明
Owner 江西汇和化工有限公司
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