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Double label <13>C2-acetic acid preparation method

A double labeling and acetic acid technology, which is applied in the preparation of carboxylate, organic compound, organic chemical methods, etc., can solve the problems of complex operation, high equipment requirements, high cost, etc., and achieve high chemical purity, simple equipment, and easy operation Effect

Active Publication Date: 2011-05-11
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: high equipment requirements, complicated operation, high-pressure reactor, and reaction at high temperature and high pressure, which has certain dangers; in addition, it needs to use expensive RhCl 3 As a catalyst, the cost is very high

Method used

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  • Double label &lt;13&gt;C2-acetic acid preparation method

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Experimental program
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Effect test

Embodiment 1

[0034] a double marker 13 C 2 -The preparation method of acetic acid, this method comprises the following steps:

[0035] (1) 13 CH 3 Synthesis of OH

[0036] Concentrated sulfuric acid was added dropwise to Ba 13 CO 3 (59.1 g, Atom% = 98.25%), resulting in 13 CO 2 Introduce into electromagnetic stirrer containing LiAlH within 3-4 hr 4 (5.7 grams), diethylene glycol diethyl ether (1L) in the reaction vessel, reaction temperature 20 ℃; Diethylene glycol monobutyl ether (540 grams) was added dropwise in the reaction mixture in 2-3 hours, reaction temperature 80 ℃, the mixture is distilled under reduced pressure, and the product is evaporated into a liquid nitrogen cooling receiver, and the distillation is repeated several times to obtain anhydrous high-purity 13 CH 3 OH (3.2 g).

[0037] (2) 13 CH 3 Synthesis of I

[0038] Get from step (1) 13 CH 3 OH (3.2 g) and red phosphorus (3.2 g) were mixed, reacted in a water bath at 0 ° C, added elemental iodine (12.7 g) ...

Embodiment 2

[0042] a double marker 13 C 2 -The preparation method of acetic acid, this method comprises the following steps:

[0043] (1) 13 CH 3 Synthesis of OH

[0044] Concentrated sulfuric acid was added dropwise to Ba 13 CO 3 (59.1 g, Atom% = 98.25%), resulting in 13 CO 2 Introduce into electromagnetic stirrer containing LiAlH within 3-4 hr 4 (17.1 grams), diethylene glycol diethyl ether (1L) in the reaction vessel, the reaction temperature -20 ° C; diethylene glycol monobutyl ether (245 grams) was added dropwise to the reaction mixture within 2-3 hours, the reaction temperature was 60 ℃, the mixture is distilled under reduced pressure, and the product is evaporated into a liquid nitrogen cooling receiver, and the distillation is repeated several times to obtain anhydrous high-purity 13 CH 3 OH (3.9 g).

[0045] (2) 13 CH 3 Synthesis of I

[0046] Take step (1) to get 13 CH 3 OH (3.2 grams) and red phosphorus (3.2 grams) were mixed, reacted in a water bath at -10 ° C,...

Embodiment 3

[0050] a double marker 13 C 2 -The preparation method of acetic acid, this method comprises the following steps:

[0051] (1) 13 CH 3 Synthesis of OH

[0052] Concentrated sulfuric acid was added dropwise to Ba 13 CO 3 (59.1 g, Atom% = 98.25%), resulting in 13 CO 2 Introduce into electromagnetic stirrer containing LiAlH within 3-4 hr 4 (57 grams), diglyme (1L) in the reaction vessel, reaction temperature -5 ℃; tetrahydrofurfuryl alcohol (178 grams) was added dropwise in the reaction mixture in 2-3 hours, reaction temperature 120 ℃, The mixture is distilled under reduced pressure, and the product is evaporated into a liquid nitrogen cooling receiver, and the distillation is repeated several times to obtain anhydrous high-purity 13 CH 3 OH (4.1 g).

[0053] (2) 13 CH 3 Synthesis of I

[0054] Take step (1) to get 13 CH 3 OH (3.2 g) and red phosphorus (3.2 g) were mixed, reacted in a water bath at 30 ° C, added elemental iodine (12.7 g) in batches, stopped after 1...

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Abstract

The invention relates to a method for preparing a double labeled <13>C2-acetic acid. The method comprises the following steps: using <13>C-carbonate as a raw material to prepare <13>CH3OH through a LiAlH4 reduction method, performing an iodination reaction to the <13>CH3OH by using phosphorous compounds and iodine elementary substances to generate <13>CH3I, and obtaining the double labeled <13>C2-acetic acid after performing grignard reaction to the <13>CH3I. Compared with the prior art, the method has the advantages of low price of the raw materials, reasonable process, avoidance of high-temperature and high-pressure condition, simple equipment and easy operation; besides, the yield up to 68 percent (by Ba<13>CO3), high chemical purity of the prepared product (more than or equal to 99 percent), and no reduced abundance.

Description

technical field [0001] The present invention relates to C-13 stable isotope compounds, in particular to a double-labeled 13 C 2 - Process for the preparation of acetic acid. Background technique [0002] C-13 stable isotopes have no radiation damage to the human body, so C-13 isotopes and their compounds (such as 13 C 2 -Acetic acid) is widely used in organic chemistry (such as chemical reaction mechanism, organic structure research), biochemistry (such as important natural product biosynthesis and structure research, enzymatic reaction mechanism research), pesticides (such as research on the mechanism of action of agricultural fertilizers and pesticides, Plant physiology research), medicine and clinical diagnosis (such as pathological experimental research), pharmacology (such as pharmacology and drug metabolism), geochemistry and environmental chemistry, and more and more applications in the detection of respiratory reagents. [0003] D.G.Ott et al. (J.Labbled Compds, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/08C07C51/15C07B59/00
Inventor 徐建飞王刚宋明鸣杜晓宁李良君
Owner SHANGHAI RES INST OF CHEM IND
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