Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for synthesizing 3,3-dimethyl-4-pentenoic acid methyl ester

A technology of methyl behenate and a synthesis method, applied in the field of synthesis of methyl behenate, can solve problems such as complicated operation, much tar, long reaction time, etc., and achieves simple operation and reaction process, less by-product tar, production short cycle effect

Active Publication Date: 2011-04-06
JIANGSU YANGNONG CHEM
View PDF5 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process operation is cumbersome, the reaction time is long, and the material is heated for a long time, resulting in a lot of tar in the rectification process, and the product yield is only about 65-85%.
CN200610048136 has mentioned a kind of pressurized synthesis process of methyl bentinate, which can increase the yield to 88%, but the equipment requirements are relatively high, and there are certain potential safety hazards in industrialized production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 1200kg (10kmol) of trimethyl orthoacetate, 1.2kg (0.0122 kmol) of anhydrous phosphoric acid and 86kg (1kmol) of isopentenol into a 2000L tank reactor in proportion at room temperature at 20°C, and the tank is connected with a Φ400×6000 In the packing separation tower, stir for 1 hour to mix evenly, open the reactor jacket steam, remove the by-product methanol and excess trimethyl orthoacetate through the separation tower temperature rise, remove the temperature of the kettle to 145°C for 3-4 hours, and maintain the temperature It remained unchanged for 2 hours, and the reaction was completed, and the remaining material was obtained by rectification to obtain the methyl bentinate product, the gas chromatography analysis content was 99.59%, and the yield was 90%.

Embodiment 2

[0021] Put 1200kg of trimethyl orthoacetate, 1.2kg of benzoic acid and 90kg of prenyl alcohol into a 2000L tank reactor in proportion at room temperature of 30°C. A Φ400×6000 packed separation tower is connected to the tank, and stirred for 0.2 hours to mix evenly. Open the jacket steam of the reaction kettle, remove by-product methanol and excess trimethyl orthoacetate through the separation tower, remove the temperature of the kettle for 3-5 hours to 150°C, and keep the temperature unchanged for 1 hour, the reaction is over, and the remaining material passes through Distillation to obtain methyl bentinate product, the gas chromatography analysis content of 99.33%, the yield of 88%.

Embodiment 3

[0023] Put 900kg of trimethyl orthoacetate, 0.9kg of anhydrous phosphoric acid and 86kg of prenol into a 2000L tank reactor in proportion at room temperature of 10°C. A Φ400×6000 packed separation tower is connected to the tank, and stirred for 1.5 hours to mix well , open the jacket steam of the reaction kettle, remove by-product methanol and excess trimethyl orthoacetate through the temperature rise of the separation tower, remove the temperature of the kettle for 3-5 hours to 140 ° C, and maintain the temperature for 2 hours, the reaction is over, and the remaining material The methyl bentinate product was obtained by rectification, the gas chromatography analysis content was 99.5%, and the yield was 89.9%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for synthesizing 3,3-dimethyl-4-pentenoic acid methyl ester, which comprises the following steps of: I) at the temperature of between 0 and 40 DEG C, uniformly mixing trimethyl orthoacetate, a catalyst and isoamyl enol in a molar ratio of 1:(0.0005-0.02):(0.1-0.5) in a reactor by stirring, and reacting for 0.2 to 2 hours to generate synthetic feed liquid of the 3,3-dimethyl-4-pentenoic acid methyl ester; and II) removing a byproduct of methanol and the excessive trimethyl orthoacetate from the synthetic feed liquid of the 3,3-dimethyl-4-pentenoic acid methyl ester obtained in the step I), rectifying the remaining materials to obtain a 3,3-dimethyl-4-pentenoic acid methyl ester product. The method for synthesizing the 3,3-dimethyl-4-pentenoic acid methyl ester has high reaction speed, short cycle, less byproduct of tar, high reaction yield of over 88 percent, high product content of over 99.5 percent and concise process, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a kind of synthetic method of compound, be specifically related to a kind of synthetic method of methyl pyridinate. Background technique [0002] Methyl bentinate, the chemical name is 3,3 dimethyl-4-pentenoic acid methyl ester, the pure product is a colorless and transparent liquid with a special pungent smell. Soluble in ethanol, ethyl acetate, ether and other organic solvents, insoluble in water; structural formula: [0003] [0004] Methyl bentinate is an important chemical raw material. It is not only used in general organic synthesis, but also as an intermediate in the synthesis of fluorine, chlorine and bromine pyrethroid pesticides in the pesticide chemical industry. Occupying an important position, in the early 1970s, the British Zeneca Company took the lead in realizing industrialized production. [0005] The literature "Research on the Synthesis of Methyl Cardyrinate" (Pesticides, Issue 09, 1996) reviewe...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/533C07C67/343
Inventor 戚明珠冯广军周世明孔勇陈亚军罗千杨凡谢邦伟花越如
Owner JIANGSU YANGNONG CHEM