Method for synthesizing trinitrophloroglucinol

A technology of trinitrophloroglucinol and phloroglucinol is applied in the synthesis field of inactive energetic material precursor trinitrophloroglucinol), and can solve the problem of corrosion equipment, complicated reaction operation, large mixed acid, etc. problems, to achieve the effect of short reaction time, easy availability of raw materials and easy handling

Active Publication Date: 2010-12-01
青岛生物能源与过程研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of synthetic method of trinitrophloroglucinol, to overcome the complex reaction operation existing in the existing production technology, a large amount of mixed acid corrodes the problems such as equipment

Method used

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  • Method for synthesizing trinitrophloroglucinol
  • Method for synthesizing trinitrophloroglucinol
  • Method for synthesizing trinitrophloroglucinol

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh phloroglucinol (0.63g, 0.50mmol) and ZrO (NO 3 ) 2 2H 2 O (4.80g, 1.50mmol) in 50mL round bottom reaction flask, add 1.0g [Hmim] [HSO 4 ] ionic liquid, stirred evenly at room temperature, reacted in an oil bath at 50°C, cooled in an ice bath after initiation, added water to dilute after reacting at room temperature for 30 minutes, extracted with ethyl acetate (3 × 20mL) and concentrated under reduced pressure, TLC analysis (acetic acid Ethyl ester: acetone = 2: 1, R f =0.5), separated by flash column chromatography (ethyl acetate: acetone = 2: 1), the product 1,3,5-trihydroxy-2,4,6-trinitrobenzene (TNPG) was obtained as light yellow crystals. The NMR spectrum of the product is as figure 1 and figure 2 As shown, the mass spectrum is as image 3 shown.

Embodiment 2

[0032] Weigh phloroglucinol (0.63g, 0.50mmol) and Bi(NO 3 ) 3 ·5H 2 O (9.70g, 2.00mmol) in 50mL round bottom reaction flask, add 2.0g [Heim] [HSO 4 ] ionic liquid, after stirring evenly at normal temperature, trigger the reaction at 60°C in an oil bath, move to normal temperature for 30 minutes after triggering, add water to dilute, extract with ethyl acetate (3 × 20mL) and concentrate under reduced pressure, TLC analysis (ethyl acetate Ester: acetone = 2:1, R f =0.5), separated by flash column chromatography (ethyl acetate: acetone = 2: 1), the product 1,3,5-trihydroxy-2,4,6-trinitrobenzene (TNPG) was obtained as light yellow crystals.

Embodiment 3

[0034] Weigh phloroglucinol (0.63g, 0.50mmol) and VO (NO 3 ) 2 (6.32g, 2.50mmol) in a 50mL round bottom reaction flask, add 3.0g [Hbim] [HSO 4 ] ionic liquid, stirred evenly at room temperature, reacted in an oil bath at 70°C, cooled in an ice bath after initiation, added water to dilute after reacting at room temperature for 1 hour, extracted with ethyl acetate (3 × 20mL) and concentrated under reduced pressure, TLC analysis (acetic acid Ethyl ester: acetone = 2: 1, R f =0.5), separated by flash column chromatography (ethyl acetate: acetone = 2: 1), the product 1,3,5-trihydroxy-2,4,6-trinitrobenzene (TNPG) was obtained as light yellow crystals.

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Abstract

The invention provides a method for synthesizing trinitrophloroglucinol. The method comprises the following steps: dissolving phloroglucinol in acid ionic fluid, wherein 1 to 50g of the acid ionic fluid is added into every 0.5 mmol of the phloroglucinol reactant; adding nitrate as nitrifier, wherein the dosage of the nitrifier is 3 to 25 times of that of the phloroglucinol substance; stirring themixture to initiate a reaction at the temperature of between 30 and 100 DEG C; reacting for 0.1 to 24 hours at normal temperature after the reaction is initiated, and cooling the mixture; and extracting the mixture with an organic solvent; and separating by column chromatography to obtain the target product. The method has the advantages of simple and convenient operation, cheap and accessible raw materials, mild reacting condition, convenient post-treatment and short reacting time, and eliminates the defects of strict condition, mixed acid corrosion on equipment and the like in the traditional synthesizing method.

Description

technical field [0001] The invention relates to a method for synthesizing trinitrophloroglucinol (1,3,5-trihydroxy-2,4,6-trinitrobenzene (TNP G)), a precursor of an insensitive energetic material. Background technique [0002] 1,3,5-Trihydroxy-2,4,6-trinitrobenzene (TNPG) is a compound with strong acidity, which can form metal salts with strong combustion or explosive properties with various metals, among which three Lead nitrophloroglucinol is an important primary explosive. In addition, it is also a synthetic insensitive, high-energy explosive 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) and a new type of explosive An intermediate of ammonium diaminopicrate (ADAP). [0003] There are many synthetic methods for trinitrophloroglucinol. At present, the route of synthesizing trinitrophloroglucinol by nitration of phloroglucinol is the most mature. The traditional process is to use the mixed acid of concentrated sulfuric acid and concentrated nitric acid as the nitrating reage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/24C07C201/08
Inventor 咸漠谭伟强李良智从琦
Owner 青岛生物能源与过程研究所
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