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Synthesis method of 7-bromotetradecane

A technology of bromotetradecane and a synthesis method, applied in the field of material synthesis, can solve the problems of difficulty in obtaining 7-bromotetradecane, inability to separate 6-bromotetradecane, and difficulty in obtaining raw materials. The effect of high product purity and mild reaction temperature

Active Publication Date: 2020-08-14
LONGXINING SHANGHAI PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this synthetic route, the raw materials are not easy to obtain, and the 6-bromotetradecane produced at the same time cannot be separated, so it is difficult to obtain pure product 7-bromotetradecane

Method used

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  • Synthesis method of 7-bromotetradecane
  • Synthesis method of 7-bromotetradecane
  • Synthesis method of 7-bromotetradecane

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preparation example Construction

[0031] The present invention provides a kind of synthetic method of 7-bromotetradecane, and its synthetic route and synthetic steps are as follows:

[0032]

[0033] Step 1, synthesis of Grignard reagents:

[0034] Magnesium is added to the reaction flask, 1-bromoheptane and tetrahydrofuran or 2-methyltetrahydrofuran are prepared into a solution, and added dropwise to the reaction flask for reaction to generate Grignard reagent;

[0035] Step 2, synthesis of 7-tetradecyl alcohol:

[0036] Add heptanal dropwise to the system after the reaction in step 1, keep the reaction for 30-60 minutes, quench the reaction with dilute hydrochloric acid, add acetic acid for extraction; then combine the organic phases, then wash the organic phases with saturated saline, and wash them with anhydrous Dry over sodium sulfate, filter, and desolventize to obtain the crude product of 7-tetradecyl alcohol;

[0037] Step three, synthesis of 7-bromotetradecane:

[0038] Dissolve the 7-tetradecyl...

Embodiment 1

[0050] The present embodiment provides a kind of synthetic method of preferred 7-bromotetradecane, comprises the following steps:

[0051] Step 1: Magnesium (2.88g, 0.12mol) is added to the reaction flask, 1-bromoheptane (17.8g, 0.1mol) and tetrahydrofuran (150ml) are prepared into a solution, which is added dropwise to the reaction flask to start the dropwise addition at room temperature After initiation, the temperature of the reaction system was lowered to 0°C, and the remaining tetrahydrofuran solution of 1-bromoheptane was continuously added dropwise, and the temperature was controlled at 0°C. After the addition was completed, the Grignard reagent was obtained by keeping the temperature at 0°C for 1 hour;

[0052] Step 2: Add heptanal (11.4g, 0.1mol) dropwise to the reaction system in Step 1, and keep the temperature below 5°C. After the addition, keep warm at 0°C for 60min, and quench with 2N dilute hydrochloric acid (150ml). The reaction was quenched, and acetic acid (3...

Embodiment 2

[0057] The present embodiment provides a kind of synthetic method of preferred 7-bromotetradecane, comprises the following steps:

[0058] Step 1, magnesium (2.88g, 0.12mol) was added to the reaction flask, 1-bromoheptane (17.8g, 0.1mol) and 2-methyltetrahydrofuran (150ml) were prepared into a solution, and added dropwise to the reaction flask Start dropwise addition at room temperature until initiation, then cool down the reaction system to 0°C, continue to dropwise add the remaining 1-bromoheptane in 2-methyltetrahydrofuran solution, control the temperature at 0°C, after the dropwise addition, keep the reaction at 0°C for 1 hour Get the Grignard reagent;

[0059]Step 2: Add heptanal (11.4g, 0.1mol) dropwise to the reaction system in Step 1, and keep the temperature below 5°C. After the addition, keep the reaction at 10°C for 40 minutes, and quench with 2N dilute hydrochloric acid (150ml). To quench the reaction, add acetic acid (3*150ml) to extract three times, combine the ...

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Abstract

The invention provides a synthesis method of 7-bromotetradecane, and the method comprises the following steps: S1, adding magnesium into a reaction bottle, preparing 1-bromoheptane and tetrahydrofuranor 2-methyltetrahydrofuran into a solution, and dropwisely adding the solution into the reaction bottle to react to generate a Grignard reagent; S2, dropwisely adding heptaldehyde to a system obtained after the reaction in the step S1, and generating 7-tetradecanol through a reaction at the temperature of 0 DEG C; and S3, dissolving the 7-tetradecanol obtained in the step S2 in hydrobromic acid,and heating to 90-110 DEG C for reaction to obtain the 7-bromotetradecane. The synthesis method of the 7-bromotetradecane provided by the invention adopts the 1-bromoheptane and the heptaldehyde as raw materials, the raw materials are easy to obtain and cheap, and the whole synthesis process is mild in reaction temperature and high in product purity, so that the method is suitable for large-scaleindustrial production and can meet market requirements.

Description

technical field [0001] The invention relates to the technical field of material synthesis, in particular to a synthesis method of 7-bromotetradecane. Background technique [0002] Intermediates refer to semi-finished products, which are intermediate products in the production of certain products. For example, if a product is to be produced, it can be produced from intermediates to save costs. Therefore, improving the yield of intermediates and optimizing their synthesis methods can greatly promote the synthesis of materials and reduce costs. [0003] 7-Bromotetradecane is an important intermediate of materials, and its chemical structure is as follows: [0004] [0005] The current main synthetic routes are as follows: [0006] [0007] 1,7-Tetradecene is added by hydrogen bromide to give 7-bromotetradecane. However, in this synthetic route, the raw materials are not easy to obtain, and the 6-bromotetradecane produced at the same time cannot be separated, so it is d...

Claims

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Application Information

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IPC IPC(8): C07C17/16C07C19/075C07C29/40C07C31/125C07F3/02
CPCC07C17/16C07C29/40C07F3/02C07C19/075C07C31/125
Inventor 彭如清李春成赵沈江朱宁
Owner LONGXINING SHANGHAI PHARMA TECH CO LTD
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