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Preparation method of adamantanone

A technology of adamantanone and adamantane, which is applied in the field of preparation of adamantane, can solve problems such as cumbersome operation process, and achieve the effects of simple operation process, high efficiency and short residence time.

Pending Publication Date: 2021-04-02
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

The production method of 2-adamantanone in the above-mentioned patent has the following disadvantages: the total reaction time is 16 hours to 27 hours, and multiple two-phase reactions and extraction operations are taken, and the operation process is cumbersome

Method used

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  • Preparation method of adamantanone
  • Preparation method of adamantanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method of adamantanone, such as figure 1 shown, including the following steps:

[0035] S1: Put the raw materials adamantane, sulfuric acid and trifluoroacetic acid into the batching kettle and stir and mix at 30°C;

[0036] S2: raise the temperature to 50°C, and feed nitrogen into the batching kettle;

[0037] S3: press the mixed material into the reaction tube, and stay for 1 minute;

[0038] S4: Pour the reaction solution onto 500 g of ice, add NaOH aqueous solution 7 times the weight of adamantane during cooling, and adjust the pH to 9;

[0039] S5: Extract with toluene 3 times the weight of adamantane, and analyze the extract by gas chromatography;

[0040] S6: Concentrate the extract to 63% by vacuum distillation, then cool, separate and dry to obtain the product.

[0041] The ratio of adamantane, sulfuric acid and trifluoroacetic acid in S1 is 1:6:2, and the concentration of sulfuric acid is ≥98%.

[0042] The preparation method of adamantane i...

Embodiment 2

[0053] A preparation method of adamantanone, such as figure 2 shown, including the following steps:

[0054] S1: Put the raw materials adamantane, sulfuric acid and trifluoroacetic acid into the batching kettle and stir and mix at 35°C;

[0055] S2: raise the temperature to 35°C, and feed nitrogen into the batching kettle;

[0056] S3: Press the mixed material into the reaction tube and stay for 40s;

[0057] S4: Pour the reaction solution into 500 g of ice water, add NaOH aqueous solution 7 times the weight of adamantane during the cooling period, and adjust the pH to 9;

[0058] S5: Extract with toluene 3 times the weight of adamantane, and analyze the extract by gas chromatography;

[0059] S6: Concentrate the extract to 62% by vacuum distillation, then cool, separate and dry to obtain the product.

[0060] The ratio of adamantane, sulfuric acid and trifluoroacetic acid in S1 is 1:6:2, and the concentration of sulfuric acid is ≥98%.

[0061] The preparation method of ad...

Embodiment 3

[0071] A preparation method of adamantanone, such as figure 1 shown, including the following steps:

[0072] S1: Put the raw materials adamantane, sulfuric acid and trifluoroacetic acid into the batching kettle and stir and mix at 30°C;

[0073] S2: raise the temperature to 50°C, and feed nitrogen into the batching kettle;

[0074] S3: press the mixed material into the reaction tube, and stay for 1 minute;

[0075] S4: Pour the reaction solution onto 500 g of ice, add NaOH aqueous solution 7 times the weight of adamantane during cooling, and adjust the pH to 9;

[0076] S5: Extract with toluene 3 times the weight of adamantane, and analyze the extract by gas chromatography;

[0077] S6: Concentrate the extract to 63% by vacuum distillation, then cool, separate and dry to obtain the product.

[0078] The ratio of adamantane, sulfuric acid and trifluoroacetic acid in S1 is 1:6:3, and the concentration of sulfuric acid is ≥98%.

[0079] The preparation method of adamantane i...

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Abstract

The invention discloses a preparation method of adamantanone, and relates to the technical field of adamantanone synthesis. The problems that the reaction time is long and the operation process is tedious are solved. The preparation method specifically comprises the following steps: putting raw materials including adamantane, sulfuric acid and trifluoroacetic acid into a batching kettle, and stirring and mixing at 30 DEG C; raising the temperature to 50 DEG C, and introducing nitrogen into the batching kettle; pressing the mixed materials into a reaction tube, and performing standing for 1 minute; pouring the reaction solution on 500g of ice, adding a NaOH aqueous solution which is 7 times the weight of adamantane during cooling, and adjusting the pH value to 9; and extracting by using methylbenzene of which the weight is 3 times that of adamantane. The raw materials are mixed and then heated, nitrogen is introduced, then an oxidation reaction occurs, the retention time and temperatureof reaction liquid in a reaction tube are controlled in the leading-out period, the reaction liquid is extracted through methylbenzene and the NaOH aqueous solution, the extraction liquid is subjected to reduced pressure distillation concentration, cooling, separation and drying treatment, the final product is obtained, the operation process is relatively simple, the reaction is controllable, andthe time is short.

Description

technical field [0001] The invention relates to the technical field of adamantanone synthesis, in particular to a preparation method of adamantanone. Background technique [0002] Adamantanone is a derivative of adamantane. From the viewpoint of effectively utilizing carbon resources, the technology of oxidatively converting hydrocarbon compounds into alcohols or ketones is a very important technology in industry. The technology of adamantanone, an important intermediate of pharmaceutical and pesticide raw materials and industrial raw materials, is known as a method of manufacturing in concentrated sulfuric acid. The industrial production of adamantanone uses adamantane or 1-adamantanol as the starting material. It is prepared by direct oxidation of concentrated sulfuric acid. In the selective preparation of adamantanone with sulfuric acid, either the reaction speed is fast, but there are heavy components of by-products, and the yield is low, or although the yield is high, t...

Claims

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Application Information

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IPC IPC(8): C07C45/28C07C45/78C07C45/80C07C45/82C07C49/453
CPCC07C45/28C07C45/78C07C45/80C07C45/82C07C2603/74C07C49/453
Inventor 刘万里李彬侯少利刘德宙
Owner 天津民祥药业有限公司
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