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Preparation method of ferrocenecarboxylic acid

A technology of ferrocene formic acid and toluene, applied in chemical instruments and methods, metallocenes, mixers with rotary stirring devices, etc., can solve problems such as oxidation of reactants, and achieve the effects of reducing the generation of impurities and improving the feeding efficiency

Pending Publication Date: 2021-06-15
安徽泽升科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above problems, the present invention proposes a method for preparing ferrocenecarboxylic acid, which solves the defect that the reactant is prone to be oxidized during the preparation and hydrolysis process of existing ferrocenecarboxylic acid

Method used

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  • Preparation method of ferrocenecarboxylic acid
  • Preparation method of ferrocenecarboxylic acid
  • Preparation method of ferrocenecarboxylic acid

Examples

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Effect test

Embodiment 1

[0038] A preparation method of ferrocenecarboxylic acid, comprising the following steps:

[0039] 1) Adding process: add toluene to the reaction kettle one by one, start stirring, add ferrocene and toluene, then vacuumize, continue stirring and pass cooling water to adjust the internal temperature to 15°C, then pass carbon dioxide gas for 30 minutes;

[0040] 2) Synthesis process: add anhydrous AlCl to the aforementioned reaction kettle 3 And continue to feed carbon dioxide gas, keep the internal temperature at 21 ℃, keep warm for 6 hours;

[0041] 3) Hydrolysis process: Add a part of crushed ice and deionized water into the hydrolysis kettle, then carefully transfer the above reaction mixture to the hydrolysis kettle for 30 minutes, use nitrogen isolation during the period, continue to add crushed ice to maintain the internal temperature of the hydrolysis Below 30°C, continue to stir for 2 hours to ensure complete hydrolysis;

[0042] 4) Filtration and water washing process: ...

Embodiment 2

[0047] A preparation method of ferrocenecarboxylic acid, comprising the following steps:

[0048] 1) Adding process: Add toluene to the reaction kettle one by one, start stirring, add ferrocene and toluene, then vacuumize, continue stirring and pass cooling water to adjust the internal temperature to 18°C, then pass carbon dioxide gas for 40 minutes;

[0049] 2) Synthesis process: add anhydrous AlCl to the aforementioned reaction kettle 3 And continue to feed carbon dioxide gas, keep the internal temperature at 23°C, and keep warm for 8 hours;

[0050] 3) Hydrolysis process: add a part of crushed ice and deionized water to the hydrolysis kettle, then carefully transfer the above reaction mixture to the hydrolysis kettle for 60 minutes, use nitrogen isolation during the period, continue to put crushed ice into it, and maintain the internal temperature of the hydrolysis Below 30°C, continue to stir for 3 hours to ensure complete hydrolysis;

[0051] 4) Filtration and water was...

Embodiment 3

[0056] Such as figure 1 , figure 2 with image 3 As shown, the hydrolysis kettle of the present invention includes a kettle body 1, a hollow stirring rod 2 is installed in the kettle body, a first stirring blade 3 is installed in the middle of the stirring rod, and a hollow stirring rod is installed at the bottom of the stirring rod. The horizontal bar 4 is used to drop crushed ice on the horizontal bar; the first driving motor 5 is installed in the center of the horizontal bar, and a pair of stirring rollers 6 arranged horizontally are respectively installed on the left and right sides of the driving motor to stir The stick is equipped with a first helical blade 7, and the first helical blades on both sides are configured to drive the crushed ice to move outward when rotating; the top of the stirring rod passes through the hydrolysis tank, and the top side of the stirring rod is equipped with The second driving motor 8, the first driven wheel 9 is housed on the described s...

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Abstract

The invention discloses a preparation method of ferrocenecarboxylic acid. The preparation method comprises the following steps: 1) feeding; 2) synthesis; 3) hydrolysis: adding a part of crushed ice and deionized water into a hydrolysis kettle, then carefully transferring the reaction mixed solution into the hydrolysis kettle for 30-60 minutes, using nitrogen for isolation during the period, continuously adding the crushed ice, keeping the hydrolysis internal temperature to be lower than 30 DEG C, and continuously stirring for 2-3 hours to ensure complete hydrolysis; 4) filtering and washing; and 5) washing. According to the invention, the nitrogen is introduced in the hydrolysis process to isolate oxygen; and the crushed ice is fed in batches, and the temperature of the hydrolysis kettle is continuously controlled, so that the materials are prevented from being oxidized before hydrolysis, and the generation of impurities is reduced.

Description

technical field [0001] The invention relates to the field of ferrocene formic acid production, in particular to a preparation method of ferrocene formic acid. Background technique [0002] At present, ferrocene (Ferrocene) is a compound with a unique sandwich structure, and ferrous ions are sandwiched between two planar rings in a staggered configuration. Ferrocene and its derivatives have their own characteristics: (1) aromaticity, which can undergo substitution reactions and are easy to modify; (2) lipophilicity, which can interact with various enzymes in the cell through the cell membrane; (3) Low toxicity, able to metabolize in vivo. Ferrocene derivatives show a wide range of pharmacological activities in the medical field, especially in the field of anti-tumor pharmacological activities: A.Rosenefeld and other studies have shown that ferrocene-modified cisplatin derivatives have a very strong inhibitory activity against leukemia, and Its nephrotoxicity is much lower t...

Claims

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Application Information

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IPC IPC(8): C07F17/02B01J19/18B01J19/00B01F13/10B01F7/18B01F7/00
CPCC07F17/02B01J19/18B01J19/0053B01J19/0066B01F27/054B01F27/90B01F33/8305B01F33/83612
Inventor 孙喜玲孙文海刘银辉张吉
Owner 安徽泽升科技有限公司
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