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Preparation method and application of trichloroacetone with high purity

A trichloroacetone, high-purity technology, applied in the field of chemical synthesis, can solve the problems of environmental pollution, a large amount of waste water, low purity of trichloroacetone, etc.

Active Publication Date: 2010-07-07
ZHEJIANG SHENGDA BIO PHARM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Industrial production also mainly uses trichloroacetone with a purity of about 50% to prepare folic acid, but due to the low purity of trichloroacetone and many impurities in the reaction product, the quality of folic acid obtained is difficult to meet the requirements of the International Pharmacopoeia
At the same time, low-purity trichloroacetone is used as the starting material, and a large amount of waste water is produced in the synthesis and refining sections of folic acid, causing great environmental pollution.
The literature Jiangsu Broadcasting University Journal, 2002, 13 (6): 57-58 reports the preparation method of high-purity trichloroacetone, which is prepared by crystallization, but only shows that it is crystallized with a special solvent, and does not give a special What is the solvent specifically, and thus can not be realized according to the narration of the literature, the yield in the literature is very low, only 45%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The preparation of trichloroacetone with a content of more than 80%:

[0013] Add content 52% trichloroacetone 50ml (about 75 grams) in 250ml flask, 50mL sherwood oil and 10ml water, stir at normal temperature for 20 minutes, then slowly mixed system is cooled to-15 ℃, a large amount of crystals are separated out in cooling process, then Control the temperature at -15°C and stir for 2 hours, filter, wash the filter cake with petroleum ether, and dry to obtain 47 g of off-white crystals with a GC content of 82% and a yield of 98.8%.

[0014] Preparation of high-purity trichloroacetone:

[0015] Add 47g of trichloroacetone and 120ml of ethyl acetate-petroleum ether (1:2) to a 250ml flask, stir at room temperature for 20 minutes, then slowly cool the mixed system to -15°C, a large amount of crystals are precipitated during the cooling process, and then Control the temperature at -15°C and stir for 2 hours, filter, wash the filter cake with ethyl acetate-petroleum ether (1...

Embodiment 2

[0017] The preparation of trichloroacetone with a content of more than 80%:

[0018] Add content 48% trichloroacetone 50ml (about 75 grams) in 250ml flask, 150mL sherwood oil and 30ml methyl alcohol, stir at room temperature for 20 minutes, then slowly mixed system is cooled to-30 ℃, a large amount of crystals are separated out in cooling process, then Control the temperature at -30°C and stir for 2 hours, filter, wash the filter cake with petroleum ether, and dry to obtain 44.5 g of off-white crystals, the content of which is 82% according to GC analysis, and the yield is 100%.

[0019] Preparation of high-purity trichloroacetone:

[0020] Add 44.5 g of trichloroacetone and 120 ml of methyl acetate-toluene (1:5) obtained above into a 250 ml flask, stir at room temperature for 20 minutes, then slowly cool the mixed system to -30 ° C, a large amount of crystals are precipitated during the cooling process, and then Control the temperature at -30°C and stir for 2 hours, filter, ...

Embodiment 3

[0022] The preparation of trichloroacetone with a content of more than 80%:

[0023] Add 50ml (about 75 grams) of trichloroacetone with a content of 52% to a 250ml flask, 25mL toluene and 5ml water, stir at room temperature for 20 minutes, then slowly cool the mixed system to 10°C, during the cooling process, a large amount of crystals are precipitated, and then control the temperature After stirring at 10° C. for 2 hours, filter, wash the filter cake with petroleum ether, and dry to obtain 47.5 g of crystals, the content of GC analysis is 82.5%, and the yield is 100%.

[0024] Preparation of high-purity trichloroacetone:

[0025] Add 47.5 g of the above-mentioned trichloroacetone and 120 ml of methyl acetate-n-hexane (1:5) to a 250 ml flask, stir at room temperature for 20 minutes, then slowly cool the mixed system to 10° C., a large amount of crystals are precipitated during the cooling process, and then Control the temperature at 10°C and stir for 2 hours, filter, wash the...

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PUM

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Abstract

The invention discloses a preparation method of trichloroacetone with high purity, which uses a solvent refining method to prepare the trichloroacetone with high purity and comprises the following two steps: step one, using mixed solvent of varsol and polar solvent for recrystallization; and step two, using mixed solvent and fatty acid ester and varsol for recrystallization to improve the purity of the trichloroacetone with low purity to above 80-98%.

Description

technical field [0001] The invention relates to a preparation method of high-purity trichloroacetone, which belongs to the field of chemical synthesis. In particular, it relates to a method for refining and preparing high-purity trichloroacetone with a solvent. Background technique [0002] Trichloroacetone is an important industrial raw material. Trichloroacetone, especially high-purity trichloroacetone, has an extremely wide range of uses and can be used in the synthesis and research of anti-HIV drugs, imidazole heterocyclic compounds, polycyclic or bridged ring compounds . Trichloroacetone is also an important intermediate in the production of folic acid. Folic acid, also known as vitamin M, belongs to the basic varieties of vitamins. Folic acid is used as an anti-anemia drug for the treatment of cellular anemia, colorectal cancer and other diseases. In food, feed and other industries, it can be used as anti-anemia drug additives, nutritional supplements, etc. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/16C07C45/63
Inventor 吴范宏肖繁花黄红军熊杨朱勇刚
Owner ZHEJIANG SHENGDA BIO PHARM
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