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The preparation method of 2-methyl-1-ethynyl-2-penten-1-ol

A technology of ethynyl and methyl, which is applied in the field of preparation of 2-methyl-1-ethynyl-2-penten-1-ol, which can solve the problems of large amount of wastewater treatment, large environmental pollution, and large production odor , to achieve the effect of high product yield, lower production cost and low production cost

Active Publication Date: 2020-06-09
JIANGSU YANGNONG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of sodium amide and liquid ammonia cannot be avoided. In industrial production, there are not only great safety hazards, but also the production smell is large, the amount of wastewater treatment is large, the ammonia nitrogen is high, and the environment is polluted.

Method used

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  • The preparation method of 2-methyl-1-ethynyl-2-penten-1-ol

Examples

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Effect test

Embodiment 1

[0035] 1, a kind of preparation method of 2-methyl-1-ethynyl-2-penten-1-alcohol, comprises the following steps:

[0036] (1) Put 48kg of magnesium chips and 1440kg of tetrahydrofuran into the reaction kettle, add 4.8kg of methylmagnesium chloride and stir at 50-60°C for Grignard initiation; Add methyl chloride at a constant speed to the system until the pressure of the system rises and the magnesium chips react completely to generate methylmagnesium chloride;

[0037] (2) Cool the methylmagnesium chloride generated in step (1) to -20—-10°C, add 0.048kg of tributylamine, and add 57.2kg of acetylene to the system at a uniform speed within 10 hours at this temperature to react, add Sampling in the process of acetylene is carried out gas chromatographic analysis, and the reaction is completed when the quality of methylmagnesium chloride in the system is less than or equal to 0.5%.

[0038] (3) Add 156.8kg of 2-methyl-2-pentenal dropwise to the system after the reaction in step (2...

Embodiment 2

[0040] 1, a kind of preparation method of 2-methyl-1-ethynyl-2-penten-1-alcohol, comprises the following steps:

[0041] (1) Put 48kg of magnesium chips and 960kg of tetrahydrofuran into the reaction kettle, add 4.8kg of methylmagnesium chloride and stir at 50-60°C for Grignard initiation; when the temperature of the system rises, the initiation begins. Add methyl chloride at a constant speed to the system until the pressure of the system rises and the magnesium chips react completely to generate methylmagnesium chloride;

[0042](2) Cool down the methylmagnesium chloride generated in step (1) to -20—-10°C, add 0.096kg of triethylamine, then add 62.4kg of acetylene to the system at a uniform speed within 10 hours at this temperature to react, add Sampling in the process of acetylene is carried out gas chromatographic analysis, and the reaction is completed when the quality of methylmagnesium chloride in the system is less than or equal to 0.5%.

[0043] (3) Add 156.8kg of 2-m...

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Abstract

The invention discloses a preparation method of 2-methyl-1-ethynyl-2-penten-1-ol, wherein the preparation method comprises the steps: firstly, introducing chloromethane into tetrahydrofuran and magnesium chips, carrying out a Grignard reaction, and generating methyl magnesium chloride; cooling, adding a catalyst, and introducing acetylene to generate acetylene magnesium chloride; and after completion of the reaction, dropwise adding 2-methyl-2-pentenal, hydrolyzing with dilute hydrochloric acid, washing an organic layer by water, carrying out reduced pressure distillation, and rectifying a residual material to obtain 2-methyl-1-ethynyl-2-penten-1-ol. The method is easy to operate, cheap and easily obtained chloromethane is used as a raw material, dangerous sodium amide or liquid ammonia isnot used, and tetrahydrofuran, toluene and other solvents can be reused, the product yield is high, the purity is high, and the cost is low.

Description

technical field [0001] The invention relates to a preparation method of 2-methyl-1-ethynyl-2-penten-1-ol, which belongs to the technical field of fine chemicals. Background technique [0002] 2-Methyl-1-ethynyl-2-penten-1-ol is a kind of "alkynyl alcohol", which is the synthesis of pentethrin (also known as fenthrin, code S-2852) and pentynethrin One of the main intermediates of new pyrethroid insecticides with high efficiency and low toxicity such as permethrin (code S-2876). The main production process is that propionaldehyde undergoes self-condensation reaction under alkali catalysis to generate 2-methyl-2-pentenal, and then reacts with sodium acetylene in liquid ammonia to generate 2-methyl-1-ethynyl-2-pentene -1-ol. The reaction formula is as follows: [0003] [0004] About the preparation of 2-methyl-1-ethynyl-2-penten-1-ol, there are few applications for invention patents at home and abroad. Since the 1980s in China, there are only sporadic reports on the synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/40C07C33/048
CPCC07C29/40C07F3/02C07C33/048
Inventor 周其奎姜友法刘静远刘卫荣张瑜蓉周世明潘学峰
Owner JIANGSU YANGNONG CHEM
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