Preparation method and storage method of 1-methyl cyclopropene lithium

A technology of lithium methylcyclopropene and methyl propylene, which is applied in the direction of lithium organic compounds, can solve problems such as instability, and achieve the effects of easy operation, stable reaction, and low production cost

Inactive Publication Date: 2014-10-08
BINHAI WEIJIA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, many patents use 1-methylcyclopropene lithium instead of 1-methylcyclopropene sodium. Although the stability of the former is better than that of the latter, it is also very unstable, so the stability problem needs to be further solved.

Method used

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  • Preparation method and storage method of 1-methyl cyclopropene lithium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example method of synthesizing 1-methylcyclopropene lithium with lithium diisopropylamide: add 100ml of 1.5mol / l lithium diisopropylamide (0.15mol) into a 250ml four-necked reaction flask, and heat to 45 degrees Celsius Then add 0.4g of catalyst hexamethyldisilazane and 0.204g of triethylamine, prepare 6.795g of 3-chloro-2-methylpropene, put it into the constant pressure funnel, and add it dropwise at a constant speed, preferably controlled within about 1 hour Addition is complete. React for 1 hour after the dropwise addition is completed. After the reaction is completed, the sample is vacuumed and distilled at a pressure of 0.1 mpa. Distill for 1 hour. The specific time is determined according to the actual situation. Take 0.3g sample in Erlenmeyer flask, then add 40ml water, shake for about 5 minutes, gas phase, analysis result gas purity is 98.43%, containing a small amount of cyclohexane.

[0020]

Embodiment 2

[0022] Synthesis of 1-methylcyclopropene lithium with lithium diisopropylamide Example method: add 100ml of 1.5mol / l lithium diisopropylamide (0.15mol) to a 250ml four-necked reaction flask, and heat to 40 degrees Celsius Then add 0.4g of catalyst hexamethyldisilazane and 0.204g of triethylamine, prepare 4.08g of 3-chloro-2-methylpropene, put it into the constant pressure funnel, and add it dropwise at a constant speed, preferably controlled within about 1 hour Addition is complete. After the dropwise addition, react for 0.5 hours. After the reaction is completed, the sample is vacuumed and distilled at a pressure of 0.1 mpa. Distill for 0.5 hours. The specific time is determined according to the actual situation. Take 0.3g sample in Erlenmeyer flask, then add 40ml water, shake for about 5 minutes, gas phase, analysis result gas purity is 98.39%, containing a small amount of cyclohexane.

[0023]

Embodiment 3

[0025] Synthesis of 1-methylcyclopropene lithium with lithium diisopropylamide Example method: Add 100ml of 1.5mol / l lithium diisopropylamide (0.15mol) into a 250ml four-necked reaction flask and heat to 50 degrees Celsius Then add 0.4g of catalyst hexamethyldisilazane and 0.204g of triethylamine, prepare 5.1g of 3-chloro-2-methylpropene and put it into a constant pressure funnel, add it dropwise at a constant speed, preferably within about 1 hour Addition is complete. React for 1 hour after the dropwise addition is completed. After the reaction is completed, the sample is vacuumed and distilled at a pressure of 0.1 mpa. Distill for 1 hour. The specific time is determined according to the actual situation. Take 0.3g sample in Erlenmeyer flask, then add 40ml water, shake for about 5 minutes, gas phase, analysis result gas purity is 98.29%, containing a small amount of cyclohexane.

[0026]

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Abstract

The invention discloses a preparation method of 1-methyle cyclopropene lithium. Reaction is carried out on organic lithium and 3-halogen-2-methyl propene under the protection of inert gas or nitrogen, then a catalyst and a structure regulator are added, and reaction is carried out at a certain temperature, so that the 1-methyl cyclopropene lithium is obtained. The invention also discloses a storage method of the 1-methyl cyclopropene lithium. The invention aims at providing the preparation method and the storage method of the 1-methyl cyclopropene lithium. The preparation method of the 1-methyl cyclopropene lithium has the advantages that raw materials are common and easily available, a technology is simple, the operation is easy, reaction is much smooth compared with sodium amide, the production cost is low, and the preparation method of the 1-methyl cyclopropene lithium can be widely used and popularized.

Description

technical field [0001] The invention relates to a preparation method of release paper, in particular to a preparation and storage method of 1-methylcyclopropene lithium. Background technique [0002] Because 1-mcp is relatively active and easy to self-polymerize and be oxidized, it is a big problem to make it stable. At present, cyclodextrin / 1-mcp inclusion compound mainly appears in the market. And this absorption process is very inefficient. The molecular weight of α-cyclodextrin is 973, and the molecular weight of 1-mcp is 54. Even if they can be fully included at a ratio of 1:1, the content of 1-mcp in the final inclusion complex is only 5.26%, but in fact we are very It is difficult to achieve 100% inclusion complexes, and inclusion compounds with a content of 3.3% generally appear on the market; after inclusion complexes are completed, they must be filtered and dehydrated, and other impurities must be washed to remove them. In this process, 1-mcp will be oxidized or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/02
Inventor 范海燕
Owner BINHAI WEIJIA CHEM
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