Method for continuously synthesizing 3,3-dimethyl-4-pentenoic acid methylester

A technology for the synthesis of methyl bentinate, which is applied in the field of continuous synthesis of methyl bentinate, can solve the problems of long reaction time, low product yield, and low reaction rate, and achieve shortening of the reaction cycle and the reduction of by-products The effect of low content and fast reaction rate

Inactive Publication Date: 2012-07-11
山东高新润农化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are following problems in this method: first what this method uses is phosphoric acid catalyst, and acidity is stronger, has certain corrosivity to equipment, and reaction rate is lower, and reaction time is longer, and by-product content is higher simultaneously, causes product yield to be relat...

Method used

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  • Method for continuously synthesizing 3,3-dimethyl-4-pentenoic acid methylester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A) Ingredients: Continuously add prenyl alcohol, trimethyl orthoacetate and phenol with a molar ratio of 1:3:0.012 to the batching kettle, and mix evenly to obtain a mixture;

[0022] B) Synthesis and separation 1: Continuously send the above-mentioned mixture to the first synthesis and separation tower for reaction, the feed temperature is controlled at 65°C, the temperature of the first synthesis and separation tower is controlled at about 80°C, The temperature is controlled at about 70°C, and the by-product methanol is continuously extracted;

[0023] C) Synthesis and separation 2: The materials in the bottom of the first synthesis and separation tower are continuously sent to the second synthesis and separation tower. At about 115°C, excess trimethyl orthoacetate is continuously distilled out;

[0024] D) Vacuum rectification: Continuously inject the material of the second synthesis separation tower into the rectification tank for vacuum distillation, the temperatu...

Embodiment 2

[0028] A) Ingredients: Continuously add isopentenol, trimethyl orthoacetate and phenol with a molar ratio of 1:3:0.005 to the batching kettle, and mix evenly to obtain a mixture;

[0029] B) Synthesis and separation 1: Continuously send the above-mentioned mixture to the first synthesis separation tower for reaction, the feed temperature is controlled at 62°C, the temperature of the first synthesis separation tower is controlled at about 80°C, the top The temperature is controlled at about 70°C, and the by-product methanol is continuously extracted;

[0030] C) Synthesis and separation 2: The materials in the bottom of the first synthesis and separation tower are continuously sent to the second synthesis and separation tower. At about 115°C, excess trimethyl orthoacetate is continuously distilled out;

[0031] D) Vacuum rectification: Continuously inject the material of the second synthesis separation tower into the rectification tank for vacuum distillation, the temperature ...

Embodiment 3

[0035] A) Ingredients: Continuously add prenyl alcohol, trimethyl orthoacetate and phenol in a molar ratio of 1:3:0.02 to the batching kettle, and mix evenly to obtain a mixture;

[0036] B) Synthesis and separation 1: Continuously send the above-mentioned mixture to the first synthesis separation tower for reaction, the feed temperature is controlled at 68°C, the temperature of the first synthesis separation tower is controlled at about 80°C, the top The temperature is controlled at about 70°C, and the by-product methanol is continuously extracted;

[0037] C) Synthesis and separation 2: The materials in the bottom of the first synthesis and separation tower are continuously sent to the second synthesis and separation tower. At about 115°C, excess trimethyl orthoacetate is continuously distilled out;

[0038] D) Vacuum rectification: Continuously inject the material of the second synthesis separation tower into the rectification tank for vacuum distillation, the temperature ...

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Abstract

The invention discloses a method for continuously synthesizing 3,3-dimethyl-4-pentenoic acid methylester and relates to a compound synthesizing technology. Methyl-2-buten-1-ol and trimethyl orthoacetate are taken as raw materials, phenol is taken as a reaction catalyst, and the method comprises the following process steps of: (A) dispensing: continuously adding the trimethyl orthoacetate, the methyl-2-buten-1-ol and the catalyst phenol into a dispensing kettle, and uniformly mixing; (B) synthesizing and separating: continuously conveying the material in the dispensing kettle to a synthesis and separation tower for reaction, continuously separating out the generated byproduct methanol and excessive trimethyl orthoacetate on the top of the tower, and continuously extracting residue at the bottom of the tower; (C) distilling at reduced pressure: continuously injecting the residue of the synthesis and separation tower into a rectifying still, distilling at reduced pressure, and separating out the finished product 3,3-dimethyl-4-pentenoic acid methylester; and (D) storing: conveying the finished product 3,3-dimethyl-4-pentenoic acid methylester to a storage tank, and standing for later use. By the method, the synthetic yield of the 3,3-dimethyl-4-pentenoic acid methylester is improved, and full continuous operation of the process for synthesizing the finished product 3,3-dimethyl-4-pentenoic acid methylester is realized.

Description

technical field [0001] The present invention relates to a kind of synthesis method of compound, in particular to a kind of continuous synthesis method of methyl pyribinate. Background technique [0002] Methyl permethrin is a colorless transparent liquid. It is an important intermediate for the synthesis of DV-methyl chrysanthemum and 2-cis-triflumethrin. Its structural formula is as follows: [0003] [0004] At present, the commonly used synthetic method of methyl pyribinate is to prepare by reacting isopentenol and trimethyl orthoacetate in the presence of a catalyst, and generate by-product methanol simultaneously. The prior art mainly adopts a batch synthesis process. [0005] Chinese patent CN102001940A provides a continuous synthesis method of methyl benzinate, which is to continuously enter trimethyl orthoacetate, catalyst and prenyl alcohol into a tank reactor for 5-60 minutes of mixed reaction to generate bentinate Synthetic feed liquid of methyl pertinate; the...

Claims

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Application Information

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IPC IPC(8): C07C69/533C07C67/343
Inventor 闫振南
Owner 山东高新润农化学有限公司
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