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Process for synthesizing 3- (or-4)-nitro o-phenylenedinitrile

A technology of nitrophthalonitrile and nitrophthalonitrile, which is applied in the field of preparation of phthalonitrile, can solve problems such as pollution, dangerous operation, and difficult post-processing of products, and achieve the effect of simple process

Inactive Publication Date: 2002-09-18
EAST CHINA UNIV OF SCI & TECH +1
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Problems solved by technology

[0006] The invention provides a kind of method for preparing 3- or 4-nitrophthalonitrile, and its synthetic route is as follows: Wherein, when preparing 3- or 4-nitrophthalimide, the present invention adopts the solvent method to replace the solid-phase baking method of the prior art, which solves the harsh reaction conditions in the prior art and the difficulty in product post-treatment and the problem that the purity of the final product is not high; at the same time, the amidation process of 3- or 4-nitrophthalimide is improved, avoiding the use of a large amount of flammable organic solvents, and solving the problem of operational danger and pollution problem

Method used

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Examples

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Embodiment 13

[0019] The preparation of embodiment 13-nitrophthalonitrile

[0020] 100g of 3-nitrophthalic acid, 32g of urea, and 250mL of nitrobenzene were mixed under stirring and slowly heated to reflux. After refluxing for 1 hour, the temperature was lowered with stirring. After cooling to room temperature, filter with suction. After drying, about 120 g was obtained, which was 85 g of light yellow crystal powder, with a yield of 93%, a purity of 99.6%, and a melting point of 194.5-195° C. (consistent with the literature value).

[0021] 85 g of 3-nitrophthalimide filter cake and 300 ml of ammonia water were mixed evenly under stirring, and the temperature was slowly raised to 45° C., and then stirred for 5 hours. After cooling to room temperature, filter with suction, and wash the filter cake with ammonia water. Vacuum drying at room temperature to constant weight yielded 75 g of white crystalline powder with a yield of 82%, a purity of 99%, and a melting point of 197°...

Embodiment 24

[0023] The preparation of embodiment 24-nitrophthalonitrile

[0024] 100g of 4-nitrophthalic acid, 32g of urea, and 250mL of nitrobenzene were mixed under stirring and slowly heated to reflux. After refluxing for 1 hour, the temperature was lowered with stirring. After cooling to room temperature, filter with suction. After drying, about 120 g was obtained, which was 85 g of light yellow crystal powder, with a yield of 93%, a purity of 99.6%, and a melting point of 203-204° C. (literature value 203° C.).

[0025] 85 g of 4-nitrophthalimide filter cake and 300 ml of ammonia water were mixed evenly under stirring, and the temperature was slowly raised to 45° C., and then stirred for 5 hours. After cooling to room temperature, filter with suction, and wash the filter cake with ammonia water. Vacuum drying at room temperature to constant weight yielded 90.5 g of white crystalline powder with a yield of 99%, a purity of 99%, and a melting point of 219° C. (co...

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Abstract

A process for preparing 3 (or 4)-nitro o-phenylenedinitrile features that a solvent method instead of solid-phase roast method is used to prepare 3 (or 4)-nitro phthaloyimine and the amidation process of 3 (or 4)-nitro phthaloymidine is improved. Its advantages are gentle reaction condition, high purity of product, high safety and less pollution.

Description

technical field [0001] The invention relates to a preparation method of phthalonitrile, in particular to a preparation method of phthalonitrile with a nitro substituent on the benzene ring. Background technique [0002] High-purity phthalocyanine is mainly used in high-tech fields as optical and electrical active functional materials, for example, 1) as an organic photoconductor for laser printing photoconductive drums and flat laser printing plates; 2) as optical recording media Used in laser discs (including VCD, DVD laser discs and computer discs); 3) As an optically active substance, it is used to prepare anti-copy toner for important documents, etc. Among them, substituted phthalocyanines are more convenient to use than unsubstituted phthalocyanines. [0003] 3- or 4-nitrophthalonitrile is a class of important intermediates for the synthesis of substituted phthalocyanines (especially high-purity phthalocyanines), and its structural formula is as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/06C07C255/51
Inventor 沈永嘉胡莹玉许煦王洪太王金友
Owner EAST CHINA UNIV OF SCI & TECH
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