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Preparation method of 1-bromoadamantane

A technology of adamantane and bromination, applied in the field of preparation of 1-bromoadamantane, can solve problems such as large environmental pollution and bromine residue, and achieve the effects of reducing residue, increasing content and avoiding bumping

Inactive Publication Date: 2020-05-15
天津民祥药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method will produce a large amount of bromine residues and cause great environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of 1-bromoadamantane, comprising the following steps:

[0019] A. Add a mixture of bromine and glacial acetic acid to the reaction vessel, keeping the temperature at 5°C; the molar ratio of bromine and glacial acetic acid is 1:7;

[0020] B. Slowly add adamantane to the reaction vessel, and finally the molar ratio of bromine to adamantane is 1:5; with the addition of adamantane, gradually increase the temperature of the mixture to 23°C, and continue stirring after the temperature rise is completed 8h; the duration of adding adamantane is 3h, and the temperature change of the mixture is proportional to the square of the amount of adamantane added;

[0021] C, add cyclohexane in the mixed solution, carry out azeotropic distillation after standing for 30min, separate residual bromine and glacial acetic acid; The adding molar weight of cyclohexane is 4 times of adamantane adding molar weight;

[0022] D. The remaining mixed solution is cooled and cryst...

Embodiment 2

[0028] This embodiment is improved on the basis of Embodiment 1. In step D1, soak the filter cake with an aqueous solution containing 15 wt% potassium sulfate and 5 wt% potassium hydroxide for 5 minutes. By improving the components of the aqueous solution, the pH value of the aqueous solution is increased, and the degree of attachment of by-products to 1-bromoadamantane crystals is reduced, thereby further improving the crystal purity after washing.

[0029] In this example, the yield of 1-bromoadamantane was 84.1 wt%, and the utilization rate of bromine was 90.1%.

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Abstract

The invention discloses a preparation method of 1-bromo adamantane. The preparation method comprises the following steps: A. adding a mixed solution of bromine and glacial acetic acid into a reactionvessel, and keeping the temperature at 5-10 DEG C; B, slowly adding adamantane into the reaction vessel, wherein the molar ratio of bromine to adamantane is 1: 3-1: 5; gradually increasing the temperature of the mixed solution to 20-25 DEG C along with the addition of adamantane, and continuously stirring for 5-8 hours after the temperature reaches 20-25 DEG C; C, adding cyclohexane into the mixedsolution, standing for 30 minutes, carrying out azeotropic distillation, and separating residual bromine and glacial acetic acid; and D, carrying out cooling and crystallization on the remaining mixed solution, and washing and drying the filter cake to obtain 1-bromoadamantane. The defects in the prior art can be overcome, and the utilization rate of bromine is increased.

Description

technical field [0001] The invention relates to the technical field of adamantane application, in particular to a preparation method of 1-bromoadamantane. Background technique [0002] Adamantane can be used in many fields such as pharmaceuticals, pesticides, lubricant products, photosensitive materials, etc., and has a wide range of uses. 1-Bromoadamantane is a commonly used intermediate. The existing preparation method is to use excess bromine to react with adamantane. This method will produce a large amount of bromine residues, which will cause great environmental pollution. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of 1-bromoadamantane, which improves the utilization rate of bromine. [0004] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows. [0005] A preparation method of 1-bromoadamantane, comprising the f...

Claims

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Application Information

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IPC IPC(8): C07C17/10C07C17/38C07C23/38
CPCC07C17/10C07C17/38C07C2603/74C07C23/38
Inventor 刘万里田长海杨浩
Owner 天津民祥药业有限公司
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