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Method for chlorination of side chain of picolines

A kind of methylpyridine, chlorination reaction technology, applied in the direction of organic chemistry, etc., can solve the problems of blocking the continued action of sodium carbonate and the failure of sodium carbonate, so as to achieve surface renewal, reduce dosage, and be beneficial to the environment and atmosphere. protective effect

Inactive Publication Date: 2011-04-20
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Japanese Patent No. 1-258662 introduces the use of sodium carbonate as an acid-binding agent. In actual experiments, it is found that as the reaction proceeds, the by-product hydrogen chloride and sodium carbonate generate sodium chloride. Due to the poor water solubility of sodium chloride, it is formed on the surface of sodium carbonate. A layer of sodium chloride coating blocks the continued action of sodium carbonate, causing sodium carbonate to fail

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a 1000ml four-necked flask, equipped with electric stirring, thermometer, chlorine gas introduction tube, reflux condenser, tail gas chlorine gas absorption device, and constant temperature water bath. Take 46.6g (0.50mol) of 2-picoline, 200ml of carbon tetrachloride, 1.0g of azobisisobutyronitrile, 50g of calcium carbonate (0.5mol), and 100g of water, and put it into the reaction flask. Under stirring at 60~65°C, 42.6g (0.6mol) of chlorine gas was introduced at a constant speed within 8 hours.

[0017] After the reaction, the resulting mixture is adjusted to PH=7.0~8.0 with sodium hydroxide solution, the water phase is separated, and the insoluble calcium carbonate in carbon tetrachloride is removed by filtration, and the obtained carbon tetrachloride phase is washed with 10% sodium hydroxide, and washed with anhydrous sulfuric acid The sodium was dried, and the solvent carbon tetrachloride was evaporated under normal pressure, and the distillation residue was detec...

Embodiment 2

[0019] In a 1000ml four-necked flask, equipped with electric stirring, thermometer, chlorine gas introduction tube, reflux condenser, tail gas chlorine gas absorption device, and constant temperature water bath. Take 46.6g (0.50mol) of 2-picoline, 1.0g of azobisisobutyronitrile, 50g (0.5mol) of calcium carbonate, and 100g of water and put it into the reaction flask. Under stirring at 60~65°C, 42.6g (0.6mol) of chlorine gas was introduced at a constant speed within 8 hours.

[0020] After the reaction, the resulting mixture was adjusted to PH=8.0~9.0 with sodium hydroxide solution, extracted twice by adding ethyl acetate 100ml×2, combining the ethyl acetate phases, drying with anhydrous sodium sulfate, distilling off the solvent ethyl acetate at normal pressure, distilling The raffinate was detected by gas chromatography, and the result was normalized analysis after removing the solvent peak: 2-methylpyridine 18.6%, 2-chloromethylpyridine 76.9%, 2-dichloromethylpyridine 1.2%, 2...

Embodiment 3

[0022] Basic magnesium carbonate was used instead of calcium carbonate, the experimental operation was the same as in Example 1, and the distillation raffinate was detected by gas chromatography, and the result was normalized analysis after removing the solvent peak: 13.1% of 2-methylpyridine, 84.6% of 2-chloromethylpyridine , 2-dichloromethylpyridine 1.3%, 2-trichloromethylpyridine 0.5%. After splitting under reduced pressure, 45.7 g (0.358 mol) of 2-chloromethylpyridine was obtained, with a yield of 71.6%.

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PUM

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Abstract

The invention relates to a method used in the picolines side chain chlorination reaction. The method adopts picolines as material, chlorination reaction is performed through charging chlorine gas under the action of radical initiator, and acid-binding agent used in the reaction is water-fast carbonate. The technology of the method reduces the disproportionating reaction occurrence of chlorine gas, reduces the quantity of carbon tetrachloride, is beneficial to lower the cost and improve the working procedure, and is beneficial to the protection of the environment and the atmospheric layer at the same time.

Description

technical field [0001] The invention relates to a method for the side chain chlorination reaction of picolines, which belongs to the field of fine chemical industry. Background technique [0002] The chlorination reaction of picoline is a free radical reaction, which is usually carried out in an inert solvent such as chlorinated hydrocarbon under the action of light or a free radical initiator. The reaction is usually easily carried out on the methyl group, and the chance of chlorination reaction on the mother nucleus is very low. Because the chlorination reaction will produce hydrogen chloride, and picoline has stronger alkalinity than chloromethyl pyridine, it is easier to generate insoluble hydrochloride precipitation with hydrogen chloride, so that the reaction cannot proceed normally, and even cause the product to further chlorinate. generation, producing polychlorinated compounds. Therefore, an acid-binding agent is required to absorb hydrogen chloride, thereby freei...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/26
Inventor 高乾善
Owner SHANDONG ANALYSIS & TEST CENT
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