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A kind of stable isotope labeling basic tender yellow o and its synthesis method

A technology of stable isotope and synthesis method, which is applied in the field of stable isotope labeling of basic bright yellow O and its synthesis, and achieves the effects of easy separation and purification, simple process route, good economy and good use value.

Active Publication Date: 2017-07-07
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no literature report on the synthesis method of stable isotope labeling basic yellow O at home and abroad

Method used

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  • A kind of stable isotope labeling basic tender yellow o and its synthesis method
  • A kind of stable isotope labeling basic tender yellow o and its synthesis method
  • A kind of stable isotope labeling basic tender yellow o and its synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] A. Stable isotope labeled methane bass-D 12 Synthesis

[0051] In the flask, press N,N-dimethylaniline-D 6 The molar ratio to paraformaldehyde (mass concentration 37%) is 2:1, and N,N-dimethylaniline-D 6 The molar ratio of urea and acetic acid is 1:1:0.1. Add urea and acetic acid in sequence, and then add distilled water with a reaction volume of 20%, stir, heat to 60°C, and react for 2 hours. After the reaction is finished, wash with water, stand for suction filtration, filter cake, wash and dry. The crude yield was 98.5%, the recrystallized yield was 94.0%, the HPLC detection purity was 99.4%, and the abundance was 99.2% atom.

[0052] B. Stable isotope labeling basic bright yellow O-D 12 Synthesis

[0053] In the flask, add stable isotope-labeled methane Bess-D 12 , then press MBASE-D 12 The molar ratio with sulfur powder is 1:2, add sulfur powder, the reaction is vacuum sealed, and ammonia gas is introduced, and the reaction temperature is controlled at 120°C...

Embodiment 2

[0055] A. Stable isotope labeled methane bass-D 12 Synthesis

[0056] In the flask, press N,N-dimethylaniline-D 6 The molar ratio to paraformaldehyde (mass concentration 37%) is 3:1, and N,N-dimethylaniline-D 6 The molar ratio of urea and sodium carbonate is 1:1.5:0.15. Add urea and sodium carbonate in sequence, and then add distilled water with a reaction volume of 20%, stir, heat to 100°C, and react for 3 hours. After the reaction is finished, wash with water, stand for suction filtration, filter cake, wash and dry. The crude yield was 95.5%, the recrystallization yield was 91.0%, the HPLC detection purity was 99.3%, and the abundance was 98.9% atom.

[0057] B. Stable isotope labeling basic bright yellow O-D 12 Synthesis

[0058] Add stable isotope-labeled methane Bess-D to the flask 12 , then press MBASE-D 12 The molar ratio with sulfur powder is 1:2.5. Add sulfur powder, seal the reaction in a vacuum, pass ammonia gas, and control the reaction temperature at 160°C....

Embodiment 3

[0060] A. Stable isotope labeled methane bass-D 12 Synthesis

[0061] In the flask, press N,N-dimethylaniline-D 6 The molar ratio to paraformaldehyde (mass concentration 37%) is 4:1, and N,N-dimethylaniline-D 6 The molar ratio of urea and acetic acid is 1:2:0.15. Add urea and acetic acid in sequence, and then add distilled water with a reaction volume of 20%, stir, heat to 140°C, and react for 5 hours. After the reaction is finished, wash with water, stand for suction filtration, filter cake, wash and dry. The crude yield was 92.5%, and the recrystallized yield was 89.0%. The HPLC detection purity was 99.6%, and the abundance was 99.2% atom.

[0062] B. Stable isotope labeling basic bright yellow O-D 12 Synthesis

[0063] Add stable isotope-labeled methane Bess-D to the flask 12 , then press MBASE-D 12 The molar ratio with sulfur powder is 1:3, add sulfur powder, the reaction is vacuum sealed, and ammonia gas is introduced, and the reaction temperature is controlled at ...

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Abstract

The present invention relates to a stable isotope-marked basic tender yellow O and a synthesis method thereof. Said stable isotope marked basic tender yellow O is basic tender yellow O marked with D or 15N or 13C. During preparation, the stable isotope D or 15N or 13C-labeled methanol and aniline are used as raw materials to synthesize stable isotope D or 15N or 13C-labeled N,N-dimethylaniline precursors, which are then condensed, sulfurized and ammoniated to make stable isotope D or 15N or 13C-labeled bases Sexually bright yellow O. Compared with the prior art, the method of the invention has the advantages of simple process route, easy synthesis, easy separation and purification of products, chemical purity of products of more than 99.0%, isotopic abundance of more than 98.0% atom, which can fully meet the requirements of trace detection in the field of food safety. The economy and use value are good, and it has a good promotion prospect.

Description

technical field [0001] The invention belongs to the technical field of isotope labeling, and relates to a stable isotope-labeled basic bright yellow O and a synthesis method thereof. Background technique [0002] Basic bright yellow O, yellow uniform powder. Soluble in cold water, easily soluble in hot water, it turns bright yellow, decomposes when boiled, turns yellow when dissolved in ethanol, its dye powder turns colorless in concentrated sulfuric acid, turns light yellow after dilution, turns orange in concentrated nitric acid, turns orange in concentrated nitric acid, oxidizes in hydrogen It becomes white precipitate in sodium solution, which is a food additive banned by the state. The chemical structure of basic yellow O determines that it is carcinogenic and has obvious toxicity to the human body. At present, both developed countries and my country prohibit the use of alkaline yellow O in the field of food processing. However, some unscrupulous businessmen add it t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/24C07C249/02C07B59/00C09B55/00
Inventor 杨维成王浩然罗勇杨超李美华盛立彦方超孙雯潘洁
Owner SHANGHAI RES INST OF CHEM IND
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