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Synthesis method of 4- nitro diheptyl phthalate

A technology of diheptyl nitrophthalate and nitrophthalic acid is applied in the synthesis field of diheptyl 4-nitrophthalate, and can solve the problems of complicated operation, expensive instruments, limited method sensitivity, etc. problem, to achieve the effect of simple synthesis route, low cost and easy application

Inactive Publication Date: 2011-10-26
LIAOCHENG UNIV
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  • Summary
  • 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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  • Synthesis method of 4- nitro diheptyl phthalate
  • Synthesis method of 4- nitro diheptyl phthalate
  • Synthesis method of 4- nitro diheptyl phthalate

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Embodiment 1

[0021] The synthetic method of embodiment 1 4-nitrophthalate diheptyl

[0022] Add n-heptanol to 4-nitrophthalic acid, the amount of which is 3:1 with the amount of 4-nitrophthalic acid, and add catalyst concentrated sulfuric acid under stirring conditions, and its amount is the same as that of 4-nitrophthalic acid The mass ratio of base phthalic acid is 2:7, stirring and reflux at 125° C., and the stirring and reflux time is 13 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 12% dropwise under stirring until the pH value of the water layer is 7.2, and the oily substance is separated After subsequent treatment, yellow oily liquid 4-nitrophthalate diheptyl ester was obtained.

Embodiment 2

[0023] The synthetic method of embodiment 2 4-nitrophthalate diheptyl

[0024] Add n-heptanol to 4-nitrophthalic acid, and the ratio of its amount to the substance of 4-nitrophthalic acid is 2:1. Add catalyst concentrated hydrochloric acid under stirring condition, the mass ratio of its dosage 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.

Embodiment 3

[0025] The synthetic method of embodiment 3 4-nitrophthalate diheptyl

[0026] Add n-heptanol to 4-nitrophthalic acid, and the ratio of its usage to the substance of 4-nitrophthalic acid is 2.5:1. Add catalyst concentrated sulfuric acid under stirring condition, the mass ratio of the amount of catalyst to 4-nitrophthalic acid is 1.5:7. Stir and reflux at 118°C for 10.5 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 13% dropwise under stirring until the pH value of the water layer is 7.0, and the oily substance is separated After subsequent treatment, yellow oily liquid 4-nitrophthalate diheptyl ester was obtained.

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Abstract

The invention discloses a synthesis method of 4- nitro diheptyl phthalate, comprising the following steps: adding heptanol in 4-nitro phthalic acid, adding a catalyst with stirring, stirring at 115-125 DEG C and refluxing, reducing pressure to distill off unreacted heptanol and water generated by the reaction, adding ice water while hot, dripping sodium carbonate solution with stirring until the PH value of the water layer is in the range of 6.5-7.2, separating grease and subsequently processing to obtain a yellowish oily liquid, 4- nitro diheptyl phthalate. The method has the advantages of simple process and low cost, and is convenient for application.

Description

technical field [0001] The invention belongs to the technical field of immunochemistry and biology of small molecular organic matter, and in particular relates to a synthesis method of 4-nitro-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 use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/57C07C201/12
Inventor 杜凌云宋于燕李娟王术皓
Owner LIAOCHENG UNIV
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