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Synthetic method for 4-amino diheptyl phthalate

A technology of diheptyl aminophthalate and diheptyl nitrophthalate, which is applied in the field of synthesis of diheptyl 4-aminophthalate, can solve the problems of expensive instruments, cumbersome operations and limited method sensitivity and other problems, to achieve the effect of low cost, simple synthesis route and easy application

Inactive Publication Date: 2011-10-26
LIAOCHENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the detection of diheptyl phthalate (DHP) environmental hormones mainly includes liquid chromatography (HPLC), gas chromatography (GC) and gas-liquid-mass spectrometry (GC-MS). Derivatization must be carried out before the determination, which makes the pretreatment of the sample very complicated, the operation is cumbersome, the equipment used is expensive, and requires skilled operators and a long analysis cycle, the sensitivity of the method is also limited, and it is difficult to adapt Field detection of diheptyl phthalate (DHP) environmental hormones and large-scale screening experiments in the laboratory, etc.

Method used

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  • Synthetic method for 4-amino diheptyl phthalate
  • Synthetic method for 4-amino diheptyl phthalate
  • Synthetic method for 4-amino diheptyl phthalate

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Embodiment 1

[0025] The synthetic method of embodiment 1 4-aminophthalate diheptyl ester

[0026] (1) Synthesis of diheptyl 4-nitrophthalate: Add 30ml of heptanol to 15g of 4-nitrophthalic acid, add 1.3ml of concentrated sulfuric acid as a catalyst under stirring conditions, and control the temperature at 120 o C, after stirring and refluxing for 12 hours, remove unreacted heptanol and water generated by reaction under reduced pressure. Pour it into ice water while it is hot, and add dropwise a 10% sodium carbonate solution with a mass fraction of 10% under stirring with a glass rod until the pH value of the water layer is neutral, then separate the oily product, extract the oily substance with absolute ethanol, and combine The extract was dried with anhydrous sodium sulfate, and then the ethanol was removed by rotary evaporation to obtain 9.75 g of diheptyl 4-nitrophthalate as a yellow oily liquid.

[0027] NMR identification of diheptyl 4-nitrophthalate:

[0028] 1 H NMR (300 MHz, CDC...

Embodiment 2

[0041] The synthetic method of embodiment 2 4-aminophthalate diheptyl ester

[0042] (1) Synthesis of diheptyl 4-nitrophthalate: Add n-heptanol to 4-nitrophthalic acid, the amount of n-heptanol and the amount of 4-nitrophthalic acid The ratio is 2:1. Add catalyst concentrated hydrochloric acid under stirring condition, the mass ratio of the amount of catalyst to 4-nitrophthalic acid is 1:7. Stir and reflux at 115°C for 10 hours. Evaporate the unreacted heptanol and the water generated by the reaction under reduced pressure, pour it into ice water while it is hot, and add a sodium carbonate solution with a mass fraction of 15% dropwise under stirring until the pH value of the water layer is 6.5, and the oily substance is separated After subsequent treatment, yellow oily liquid 4-nitrophthalate diheptyl ester was obtained;

[0043] (2) Synthesis of diheptyl 4-aminophthalate: add toluene to diheptyl 4-nitrophthalate, the mass ratio of toluene to diheptyl 4-nitrophthalate is 30...

Embodiment 3

[0044] The synthetic method of embodiment 3 4-aminophthalate diheptyl ester

[0045] (1) Synthesis of diheptyl 4-nitrophthalate: Add n-heptanol to 4-nitrophthalic acid, the amount of n-heptanol and the amount of 4-nitrophthalic acid The ratio is 3:1. Add catalyst concentrated sulfuric acid under stirring condition, the mass ratio of the amount of catalyst to 4-nitrophthalic acid is 2:7. Stir and reflux at 125°C for 13 hours. The unreacted heptanol and the water generated by the reaction were evaporated under reduced pressure, poured into ice water while it was hot, and a sodium carbonate solution with a mass fraction of 12 was added dropwise with stirring until the pH value of the water layer was 7.2, and the oil was separated by Subsequent processing to obtain yellow oily liquid 4-nitro-diheptyl phthalate;

[0046] (2) Synthesis of diheptyl 4-aminophthalate: Add benzene to diheptyl 4-nitrophthalate, and the mass ratio of benzene to diheptyl 4-nitrophthalate is 24 :1. Add...

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Abstract

The invention discloses a synthetic method for 4-amino diheptyl phthalate. The method is characterized in that: 4-nitro phthalic acid is adopted as a raw material, and is subjected to a esterification with heptanol to prepare 4-nitro diheptyl phthalate; a nitro group is introduced into a benzene ring of the 4-nitro diheptyl phthalate, then the nitro group is subjected to a reduction reaction to obtain a active amino capable of combination with proteins to synthesize the 4-amino diheptyl phthalate. The method provided by the present invention has advantages of simple route, low cost and convenient application.

Description

technical field [0001] The invention belongs to the technical field of immunochemistry and biology of small molecule organic matter, and in particular relates to a synthesis method of 4-amino-diheptyl phthalate in the process of preparing diheptyl phthalate complete antigen. Background technique [0002] As a main plasticizer, diheptyl phthalate (DHP) is used in plastics, rubber, cosmetics, spices, printing and dyeing, coatings and other industries, and diheptyl phthalate (DHP) is also an environmental Estrogen, research in recent years has found that diheptyl phthalate (DHP) can pollute the environment, organisms and food. It can be absorbed by the human body through diet, breathing and skin penetration, and it is mainly harmful to the human body. Diheptyl phthalate (DHP) has estrogen-like activity, and a small amount can damage the human reproductive system, leading to testicular atrophy, hypospadias, and reduced sperm activity. There are about 14 kinds of phthalates used...

Claims

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Application Information

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IPC IPC(8): C07C229/62C07C227/04
Inventor 王术皓宋于燕庞玉波张霞
Owner LIAOCHENG UNIV
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