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Preparation method of branched alkane

A branched-chain alkane and alkyl alcohol technology, which is applied in the field of branched-chain alkane preparation, can solve the problems of inability to recycle, high equipment requirements, and large dosage, and meets the requirements of less by-products, mild reaction conditions, and equipment corrosion resistance. low effect

Inactive Publication Date: 2019-12-20
DALIAN CHEMPHY CHEM
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Problems solved by technology

[0006] The yield of this method is 24-56%, but it needs to be carried out under high temperature (180-200 ℃) and tube sealing conditions, which requires high equipment; at the same time, the catalyst used in this method is expensive, the consumption is large and cannot be recovered Therefore, it is impossible to achieve industrial mass production

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  • Preparation method of branched alkane
  • Preparation method of branched alkane
  • Preparation method of branched alkane

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preparation example Construction

[0024] The present invention provides a method for preparing branched alkanes, including the following steps:

[0025] Under protective atmosphere, mixing pinacolone, metal alkyl reagent and organic solvent, and then carry out alkylation reaction to obtain alkyl alcohol intermediate;

[0026] Under the protective atmosphere, the alkyl alcohol intermediate, the alkyl silane, the acid catalyst and the organic solvent are mixed and then subjected to elimination reduction reaction to obtain branched alkanes.

[0027] In the present invention, under the protective atmosphere, the pinacolone, the alkyl metal reagent and the organic solvent are mixed and then the alkylation reaction is carried out to obtain the alkyl alcohol intermediate. In the present invention, the alkyl metal reagent preferably includes alkyl lithium or alkyl Grignard reagent; the alkyl group in the alkyl metal reagent preferably includes methyl, ethyl, propyl or butyl; specifically, The alkyl metal reagent preferably ...

Embodiment 1

[0041] (1) Synthesis of 2,3,3-trimethylbutanol

[0042] Install a dropping funnel and argon protection device on the jacketed four-neck flask, and use argon protection for the reaction system; add a diethoxymethane solution of pinacolone (from 0.225mol pinacolone and 75mL) to the dropping funnel Mix diethoxymethane), add methyllithium diethoxymethane solution (198mL, of which the concentration of methyllithium is 1.6mol / L) into a four-necked jacketed flask with a syringe, and cool to -10℃ , Add the diethoxymethane solution of pinacolone dropwise to the four-neck jacketed flask to control the temperature of the system to be lower than -5°C; after the dropwise addition, carry out the alkylation reaction for 6h ( During the reaction, samples were taken for GC detection, and the reaction process was monitored by detecting the conversion of raw materials and the formation of products); after the alkylation reaction was completed, saturated chlorination was added to the obtained alkyla...

Embodiment 2

[0049] (1) Synthesis of 2,3,3-Trimethylpentanol

[0050] Install a dropping funnel and argon protection device on the jacketed four-necked flask, and use argon protection for the reaction system; add pinacolone tetrahydrofuran solution (from 0.225mol pinacolone and 75mL tetrahydrofuran) into the dropping funnel , Add ethyl lithium tetrahydrofuran solution (250 mL, the concentration of ethyl lithium is 1.6 mol / L) into the four-necked jacketed flask with a syringe, cool to -10℃, and add pinnacle dropwise to the four-necked jacketed flask The tetrahydrofuran solution of ketone, control the temperature of the system to be lower than -5°C; after the addition is complete, carry out the alkylation reaction for 6h under stirring and holding at 0°C (sample during the reaction for GC detection, by detecting the conversion of raw materials and the formation of products If the situation, monitor the progress of the reaction); after the alkylation reaction is completed, add a saturated aqueou...

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Abstract

The invention provides a preparation method of branched alkane, and belongs to the technical field of organic synthesis. The preparation method of the branched alkane comprises the following steps: mixing pinacolone, an alkyl metal reagent and an organic solvent under the condition of a protective atmosphere, performing an alkylation reaction so as to obtain an alkyl alcohol intermediate, mixing the alkyl alcohol intermediate, alkyl silane, an acid catalyst and an organic solvent under the condition of a protective atmosphere, and then performing an elimination reduction reaction so as to obtain the branched alkane. Pinacolone is adopted as a raw material, the alkyl metal reagent is applied to the alkylation reaction so as to obtain the corresponding alkyl alcohol intermediate, the alkyl silane is adopted as a reducing agent of the alkyl alcohol intermediate, and the elimination reduction reaction is performed in the presence of the acid catalyst so as to synthesize the branched alkane. The method has a simple synthesis route, high yield of branched alkane, high purity, no use of expensive catalysts, low raw material cost and simple operation, and is suitable for scale-up and industrial production.

Description

Technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing branched alkanes. Background technique [0002] At present, people's requirements for energy environmental protection are gradually increasing, and oil quality is a very important factor in energy environmental protection. Therefore, it is necessary to develop petroleum products with high performance and meet environmental protection requirements. A lot of research and development work has been carried out in this area at home and abroad. One of the solutions is to increase the content of branched chain alkanes in the downstream products of petroleum. With the increase of the content of branched chain alkanes, the combustion performance of the downstream products of petroleum can be significantly improved. The calorific value of oil products and the combustion stability of oil products have been correspondingly improved. This can save fuel consumption,...

Claims

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Application Information

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IPC IPC(8): C07C1/22C07C9/16
CPCC07C1/22C07C29/40C07C9/16C07C31/125
Inventor 王智勇马晓爽马建华赵宏徐海珍
Owner DALIAN CHEMPHY CHEM
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