Stable isotope labeled benzyl butyl phthalate and synthesis method thereof

A technology of butyl benzyl phthalate and monobenzyl phthalate, which is applied in the field of stable isotope labeling of butyl benzyl phthalate and its synthesis, to achieve less by-products, mild reaction conditions, and less catalyst consumption Effect

Inactive Publication Date: 2015-08-26
SHANGHAI RES INST OF CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no reports on the synthesis of isotope-labeled butyl benzyl phthalate at home and abroad. The successful development of stable isotope-labeled butyl benzyl phthalate will provide a standard reagent for more accurate quantitative detection of butyl benzyl phthalate , so as to effectively provide testing services for my country's food safety field

Method used

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  • Stable isotope labeled benzyl butyl phthalate and synthesis method thereof
  • Stable isotope labeled benzyl butyl phthalate and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] A stable isotope labeled butyl benzyl phthalate-D 4-Phenyl preparation method, this method comprises the following steps:

[0042] 1. Stable isotope labeled monobenzyl phthalate-D 4 - Preparation of phenyl

[0043] Add 15g of phthalic anhydride-D in a 250mL three-neck flask 4 , add 11g of benzyl alcohol, stir and disperse, react at 50°C for 4 hours, separate and purify to obtain 24.0g of monobenzyl phthalate-D 4 -Phenyl white solid, yield 97.5%, GC detection, purity 99.5%; mass spectrometry detection, abundance 99.3atom%D.

[0044] 2. Stable isotope labeling of butyl benzyl phthalate-D 4 - Preparation of phenyl

[0045] Add 5.1g of monobenzyl phthalate-D to a 100mL three-necked flask 4 , add 10mL butanol, 0.1g 4-dimethylaminopyridine, control the temperature at 30°C, react for 4 hours, separate and purify to obtain 5.79g butyl benzyl phthalate-D 4 -Phenyl is a colorless liquid with a yield of 96.3%, a purity of 99.5% detected by GC, and an abundance of 99.3 atom%...

Embodiment 2

[0047] A stable isotope labeled butyl benzyl phthalate-D 2 - method for the preparation of benzyl, the method comprising the steps of:

[0048] 1. Stable isotope labeled monobenzyl phthalate-D 2 - Preparation of Benzyl

[0049] Add 14.8g of phthalic anhydride in a 250mL three-necked flask, add benzyl alcohol-D 2 12.1g, stirred and dispersed, reacted at 30°C for 5 hours, separated and purified to obtain 25.2g monobenzyl phthalate-D 2 White solid, yield 98.6%, GC detection, purity 99.2%; mass spectrometry detection, abundance 99.2atom%D.

[0050] 2. Stable isotope labeling of butyl benzyl phthalate-D 2 - Preparation of Benzyl

[0051] Add 5.2g monobenzyl phthalate-D to a 100mL three-neck flask 2 , add 8 mL of butanol, 0.2 g of potassium tert-butoxide, control the temperature at 0°C, react for 8 hours, separate and purify to obtain 5.9 g of butyl benzyl phthalate-D 2 - Benzyl colorless liquid, yield 93.9%, GC detection, purity 99.5%; mass spectrometry detection, abundance ...

Embodiment 3

[0053] A stable isotope labeled butyl benzyl phthalate-D 2 -The preparation method of butyl, the method comprises the following steps:

[0054] 1. Preparation of monobenzyl phthalate

[0055] Add 7.5g of phthalic anhydride to a 50mL three-necked flask, add 5g of benzyl alcohol, stir and disperse, react at room temperature for 8 hours, separate and purify to obtain 12.0g of monobenzyl phthalate as a white solid, yield 93.5%, GC Detection, purity 99.4%.

[0056] 2. Stable isotope labeling of butyl benzyl phthalate-D 2 - Preparation of butyl

[0057] Add 6.5g monobenzyl phthalate to a 100mL three-necked flask, add 4.8mL butanol-D 2 , after stirring and dispersing, add 0.2g of diisopropylethylamine, react at room temperature for 8 hours, separate and purify to obtain 7.4g of butyl benzyl phthalate-D 2 -Butyl colorless liquid, yield 94.5%, GC detection, purity 99.3%; mass spectrometry detection, abundance 99.7atom%D.

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Abstract

The invention relates to a stable isotope labeled benzyl butyl phthalate and a synthesis method thereof. According to the invention, an organic synthesis method is adopted; stable isotope labeled phthalic anhydride is adopted as a raw material, and is subjected to a reaction with benzyl alcohol, such that stable isotope labeled monobenzyl phthalate is produced; the stable isotope labeled monobenzyl phthalate is subjected to a reaction with butanol, such that stable isotope labeled benzyl butyl phthalate is obtained. Compared with the prior art, when the stable isotope labeled benzyl butyl phthalate is separated and purified, a chemical purity can be higher than 99%, and an isotope abundance is higher than 99%, such that the demand of the detection of the illegal additive benzyl butyl phthalate in the field of food safety can be fully satisfied.

Description

technical field [0001] The invention relates to a stable isotope labeling method, in particular to a stable isotope labeled butyl benzyl phthalate and a synthesis method thereof. Background technique [0002] Butyl benzyl phthalate, the English name Benzyl butyl phthalate (BBP), is a plasticizer with certain toxicity and strong solubility. It can be mixed with polyvinyl chloride resin, vinyl acetate resin, polystyrene, nitrocellulose It has good mutual solubility, good pollution resistance, fast plasticizing speed, large filler capacity, water resistance and oil extraction resistance. Butyl benzyl phthalate can be used as the main plasticizer, and it is often used in combination with other plasticizers for plastic floors, decorative materials, corrugated boards, films, plates and pipes that contain a large amount of fillers, and can obtain excellent Products with transparency and smooth surface. [0003] However, a large number of experiments have proved that BBP has a str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/83
CPCC07C67/08C07B59/00C07B2200/05C07C69/82
Inventor 徐仲杰孙雯涂亚辉钟佳琪李美华卢浩邓晓军
Owner SHANGHAI RES INST OF CHEM IND
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