High-efficiency method for synthesizing adamantane

A synthetic method, adamantane technology, applied in the field of catalytic synthesis of fine chemicals

Active Publication Date: 2019-07-12
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Invention patent CN 1762927A uses solid superacid ZrO2-SO4 or molecular sieve solid superacid loaded with ZrO2-SO4 on the surface as a catalyst. Although adamantane is also obtained, the yield of adamantane is only 20%.

Method used

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  • High-efficiency method for synthesizing adamantane
  • High-efficiency method for synthesizing adamantane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 500 grams of trimethyl phosphate, 5 grams of phosphorus oxychloride, 10 grams of molybdenum chloride, 6 grams of manganese chloride, and 4 grams of iridium chloride into the 1000 ml reactor. After stirring and dissolving, add bridged tetrahydrobicyclic 100 grams of pentadiene, the temperature in the reactor rises to 200 ℃ from normal temperature in two hours, after reacting for 5 hours, sampling analysis, when the adamantane content is greater than 80% (not counting the amount of solvent, auxiliary agent), reduce the reaction temperature to Stir at -10°C for 9 hours, filter and rinse with 50 g of trimethyl phosphate at -10°C, blow the filter cake with air, and dry at 100°C to obtain 62 g of adamantane with a content of 99.1%.

Embodiment 2

[0020] Obtain 590 grams of mother liquor from embodiment 1, add 1 gram of phosphorus oxychloride, 62 grams of bridged tetrahydrodicyclopentadiene, after stirring and dissolving, the temperature in the reactor rises to 200 ℃ from normal temperature in two hours, reacts Sampling and analysis after 5 hours, when the adamantane content was greater than 80% (excluding the amount of solvent and auxiliary agent), reduce the reaction temperature to -10°C, stir for 9 hours, filter and wash with 50 grams of trimethyl phosphate at -10°C, After the filter cake was purged with air, it was dried at 100° C. to obtain 61 g of adamantane with a content of 99.0%.

Embodiment 3

[0022] Add 400 kg of triethyl phosphate, 5 kg of phosphorus trichloride, 14 kg of molybdenum chloride, 4 kg of manganese chloride, and 2 kg of iridium chloride into the 1000-liter reactor. After stirring and dissolving, add bridged tetrahydrobicyclic 120 kilograms of pentadiene, the temperature in the reactor rises to 200 ℃ from normal temperature in two hours, reacts sampling analysis after 5 hours, when adamantane content is greater than 80% (not counting the amount of solvent, auxiliary agent), reduce reaction temperature to Stir at -10°C for 9 hours, filter and rinse with 60 kg of triethyl phosphate at -10°C, purify the filter cake with nitrogen, and dry at 100°C to obtain 75 kg of adamantane with a content of 99.1%.

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Abstract

The invention discloses a high-efficiency method for synthesizing adamantane. According to the method, endo-tetrahydrodicyclopentadiene is adopted as a raw material, anhydrous molybdenum pentachloride, anhydrous manganese dichloride, anhydrous iridium chloride or anhydrous cerium chloride are adopted as a composite catalyst, phosphorus oxychloride and phosphorus trichloride are adopted as auxiliary agents, and trimethyl phosphate, triethyl phosphate and other phosphate are adopted as solvents so as to prepare the adamantane through catalysis. Due to the characteristics of adamantane, the raw materials, the catalysts and the solvents, the product can be precipitated in the solvents, and unconverted raw materials, intermediates and catalysts can be reused in the solvents.

Description

technical field [0001] The invention relates to an efficient method for synthesizing adamantane, which belongs to the field of catalytic synthesis of fine chemicals. Background technique [0002] In medicine, adamantane is mainly used in the synthesis of drugs such as anti-cancer, anti-tumor, and influenza caused by A2 virus, in the application of catalyst synthesis, in lubricants, and in functional polymers, pesticides, photosensitive materials, surface Applications in fields such as active agents are called a new generation of fine chemicals. [0003] In 1956, American scientists first used aluminum trichloride to catalyze bridged tetrahydrodicyclopentadiene to synthesize adamantane. Due to the strong acidity of aluminum trichloride, it is easy to cause tetrahydrodicyclopentadiene to break bonds and polymerize to form tar, so that the yield of adamantane is low. CN103406151B invention patent transforms aluminum trichloride through phenol etc., thereby passivating the cat...

Claims

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Application Information

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IPC IPC(8): C07C5/29C07C13/615
CPCC07C5/29C07C2523/34C07C2603/74C07C13/615
Inventor 郑学胜王庆吉杨晓旭王贤彬王炳春李进
Owner CHINA CATALYST HLDG CO LTD
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