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Synthetic method of stable isotope deuterium-labeled DDT

A technology of stable isotope and synthesis method, which is applied in the field of synthesis of stable isotope internal standard substances, can solve the problems of expensive reaction raw materials, difficult to obtain isotope precursors, etc., achieves good economy and use value, simple process route, avoids abundant degree of dilution

Inactive Publication Date: 2015-04-29
SHANGHAI RES INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent discloses the synthesis method of carbon-13-labeled DDT, DDD and DDE, but compared with the synthesis of stable isotope deuterium-labeled DDT, the price of reaction raw materials is relatively expensive, and the carbon-13-labeled isotope precursor is difficult to obtain, so deuterium-labeled synthesis The DDT reasonably solves the problem of economy in the experimental process on the basis of it

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  • Synthetic method of stable isotope deuterium-labeled DDT
  • Synthetic method of stable isotope deuterium-labeled DDT
  • Synthetic method of stable isotope deuterium-labeled DDT

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Experimental program
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Effect test

Embodiment 1

[0040] 23.6g stable isotope labeled chlorobenzene-D 5 Mix with 14.7g of chloral, add an appropriate amount of solvent pentane, slowly add 76.6g of oleum dropwise at 25°C, raise the temperature to 85°C after the addition, stir and react for 12h, after the reaction, the product is separated and purified After that, 17.2g of stable isotope labeled DDT-D was obtained 8 (Ⅰ). Chlorobenzene-D 5 The total yield was 45.3%. The product was detected by liquid chromatography and mass spectrometry. The purity was 99.2%, and the abundance was 99.0% atomD.

Embodiment 2

[0042] 34.1g stable isotope labeled chlorobenzene-D 5Mix with 14.7g of chloral, add an appropriate amount of solvent dichloromethane, slowly add 97.6g of 98% concentrated sulfuric acid dropwise at 25°C, raise the temperature to 50°C after the addition, stir and react for 24h, after the reaction, the product passes through After separation and purification, 35.0 g of stable isotope deuterium-labeled DDT-D was obtained 8 (Ⅰ). Chlorobenzene-D 5 The total yield was 68.7%. The product was detected by liquid chromatography and mass spectrometry. The purity was 99.3%, and the abundance was 99.1% atomD.

Embodiment 3

[0044] 45.0g stable isotope labeled chlorobenzene-D 5 Mix with 14.7g of chloral, add an appropriate amount of solvent toluene, slowly add 119.4g of oleum dropwise at 25°C, raise the temperature to 120°C after the dropwise addition, and stir for 4 hours. After the reaction, the product is separated and purified Obtain 26.4g stable isotope labeled DDT-D 8 (Ⅰ). Chlorobenzene-D 5 The total yield was 36.4%. The product was detected by liquid chromatography and mass spectrometry. The purity was 99.3%, and the abundance was 99.3% atomD.

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Abstract

The invention relates to a synthetic method of stable isotope deuterium-labeled DDT. The synthetic method comprises the following steps: with stable isotope deuterium-labeled chlorobenzene as an isotope-labeled precursor, in the presence of a catalyst, carrying out dehydration synthesis on the isotope-labeled precursor and chloral to obtain the stable isotope deuterium-labeled DDT. Compared with the prior art, according to the synthetic method disclosed by the invention, after the stable isotope deuterium-labeled DDT is separated and purified, the isotope-labeled position is stable, so that the abundance of an isotope is prevented from diluting, the chemical purity achieves above 99.0 percent, the abundance of the isotope achieves above 99.0 percent atom, and the stable isotope deuterium-labeled DDT can fully meet the needs for residue detection in the food safety field.

Description

technical field [0001] The invention relates to a synthesis method of a stable isotope internal standard substance, in particular to a synthesis method of a stable isotope deuterium-labeled DDT. Background technique [0002] DDT (DDT), chemical name: 2,2-bis(4-chlorophenyl)-1,1,1-trichloroethane, English name: 2,2-bis(4-Chlorophenyl)-1,1, 1-trichloroethane. Its main isomers and homologues are: o, p'-DDT; p, p'-DDE; p, p'-DDD, the molecular formula is C 14 h 9 C 15 . In the first half of the 20th century, DDT played a significant role in the prevention and control of agricultural pests and diseases, such as malaria and typhoid fever. The World Health Organization estimates that the use of DDT has saved approximately 25 million lives. But after the 1960s, scientists discovered that DDT is very difficult to degrade in the environment and can accumulate in animal fat, especially the carnivorous birds at the top of the food chain, such as the American national bird, the bal...

Claims

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Application Information

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IPC IPC(8): C07C25/20C07C17/263
Inventor 杨维成吕靖罗勇杨超盛立彦李美华孙雯潘洁宋家龙
Owner SHANGHAI RES INST OF CHEM IND
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