Synthesis method of 5,5,5-trichloro-2-methyl-2-pentene

A synthetic method, methyl technology, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve the problems of high reaction cost and high environmental pollution, reduce corrosion, reduce pollution, and increase chemical yield Effect

Active Publication Date: 2019-06-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two methods all have the disadvantages of high reaction cost, high environmental pollution and serious equipment corrosion

Method used

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  • Synthesis method of 5,5,5-trichloro-2-methyl-2-pentene
  • Synthesis method of 5,5,5-trichloro-2-methyl-2-pentene

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 50.0 g of 3-methyl-2-buten-1-ol into a 500.0 ml four-neck flask, drop the temperature to 0°C, add 88.4 g of 36% hydrochloric acid dropwise, stir at room temperature for 1 hour after the dropwise addition, and let stand to separate layers. The organic layer was dried over anhydrous sodium sulfate, and 52.0 g of an intermediate product was distilled off under reduced pressure.

[0018] In a 250.0 milliliter four-necked flask, add 20.0 grams of intermediate product, 100 milliliters of tetrahydrofuran, 10.7 grams of calcium oxide, 45.7 grams of chloroform, add 9.2 grams of sodium hydroxide under 0 degree stirring state, after gas chromatography tracking analysis, after the completion of the reaction, filter, the mother liquor After the solvent was removed under pressure, 28.1 g of the product 5,5,5-trichloro-2-methyl-2-pentene was distilled out, with a yield of 78%.

Embodiment 2

[0020] Add 50.0 g of 3-methyl-2-buten-1-ol into a 500.0 ml four-neck flask, drop the temperature to 0°C, add 88.4 g of 36% hydrochloric acid dropwise, stir at room temperature for 1 hour after the dropwise addition, and let stand to separate layers. The organic layer was dried over anhydrous sodium sulfate, and 52.0 g of an intermediate product was distilled off under reduced pressure.

[0021] Add 20.0 grams of intermediate product, 100 milliliters of N,N-dimethylformamide, 10.7 grams of calcium oxide, and 45.7 grams of chloroform into a 250.0 milliliter four-neck flask, add 12.8 grams of potassium hydroxide under stirring at 0 degrees, and follow up the analysis by gas chromatography After the reaction was completed, the mother liquor was filtered and the solvent was removed under reduced pressure, and 29.2 g of the product 5,5,5-trichloro-2-methyl-2-pentene was distilled out, with a yield of 81%.

Embodiment 3

[0023] Add 50.0 grams of 3-methyl-2-buten-1-ol into a 500.0 ml four-neck flask, drop the temperature to 0°C and add 140.0 grams of 40% hydrobromic acid dropwise, stir at room temperature for 1 hour after the dropwise addition, and let stand to separate layers . The organic layer was dried over anhydrous sodium sulfate, and 60.0 g of the intermediate product was distilled off under reduced pressure.

[0024] In a 250.0 milliliter four-necked flask, add 20.0 grams of intermediate product, 100 milliliters of tetrahydrofuran, 15.0 grams of calcium chloride, 45.7 grams of chloroform, add 6.5 grams of sodium hydride under stirring state at 0 degrees, after gas chromatography tracking analysis, filter, and the mother liquor reduces After the solvent was removed under pressure, 28.8 g of the product 5,5,5-trichloro-2-methyl-2-pentene was distilled out, with a yield of 80%.

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Abstract

The invention provides a synthetic method of 5,5,5-trichloro-2-methyl-2-pentene. The synthetic method comprises the following steps: taking 2-methyl-3-butene-2-ol as an initial compound of a reaction;adding a haloid acid into the reaction system, and conducting distilling to obtain an intermediate product 1-halo-3-methyl-2-butene; adding the intermediate product and chloroform into a reaction kettle, conducting stirring at a low temperature, and adding an inorganic base into the system in batches; wherein the reaction temperature is 0-40 DEG C, the reaction time is 2-10 hours, the mass ratioof the 2-methyl-3-butene-2-ol to the haloid acid in the reaction is (0.3-1):1, the weight ratio of the chloroform to the 1-halo-3-methyl-2-butene is (1-10):1, and the weight ratio of the inorganic base to the 1-halo-3-methyl-2-butene is (0.1-2.0):1. The method is high in reaction yield and low in environmental pollution degree, and the corrosion degree of equipment is reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of 5,5,5-trichloro-2-methyl-2-pentene. Background technique [0002] There are two main methods for the existing production of 5,5,5-trichloro-2-methyl-2-pentene, 1. DE2616528A1 through 2-methyl-3-butene-2-alcohol The reaction under the catalysis of toluenesulfonic acid gave a yield of 78%; 2.Jpn.Kokai Tokkyokoho, 52000207,05Jan 1977 3-Chloro-3-methyl-butene reacted with bromotrichloromethane. The above two methods all have the disadvantages of high reaction cost, high environmental pollution and serious equipment corrosion. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of 5,5,5-trichloro-2-methyl-2-pentene, its reaction raw material is simple and easy to get, widely used in the market, cost is low, and environmental pollution is relatively Low. [0004] The invention provides a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C21/04C07C21/14C07C21/17C07C17/269
Inventor 胡向平陈松
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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