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
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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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