Chemical synthetic method for n-butyryl chloride

A technology for n-butyryl chloride and chemical synthesis, which is applied in the field of green chemical synthesis of n-butyryl chloride, can solve the problems of difficult treatment of phosphorus-containing wastewater, low product yield and purity, serious equipment corrosion, etc., and achieves low production cost and three wastes. Small, high reaction yield effect

Inactive Publication Date: 2011-09-28
湖州沙龙化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The product obtained by the phosphorus trichloride process contains a large amount of by-product phosphorous acid, and phosphorus trichloride, as a chlorinated reagent, severely corrodes the equipment, and a large amount of phosph

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 125ml three-necked flask equipped with a thermometer, reflux condenser and mechanical stirring, add 8.8g (0.1mol) of n-butyric acid, 10.1g (0.034mol) of bis(trichloromethyl)carbonate, 40ml of toluene and tetramethyl Guanidine 0.1g (0.001mol), after the addition, the temperature was raised to 80°C, and reacted at 80-85°C for 5h. After the reaction was completed, the fraction at 100-110°C was collected by distillation to obtain 9.4g of n-butyryl chloride, and the product yield was 88%. 98.5% purity.

Embodiment 2

[0021] Put the following substances into the reactor: 88g (1mol) of n-butyric acid, 148.5g (0.5mol) of bis(trichloromethyl) carbonate, 1g (0.01mol) of catalyst; the catalyst is 1,3-dimethyl Base-2-imidazolidinone, the organic solvent is toluene, and its consumption is 2 times of the quality of n-butyric acid.

[0022] The reaction temperature was 60-65°C, and the reaction was carried out for 6 hours. After the reaction was completed, the fraction at 100-110°C was collected by distillation to obtain 95g of n-butyryl chloride, with a product yield of 89.2% and a purity of 99.0%.

Embodiment 3

[0024] Put the following substances into the reactor: 88g (1mol) of n-butyric acid, 101g (0.34mol) of bis(trichloromethyl)carbonate, 1g (0.01mol) of catalyst; the catalyst is pyridine, and the organic solvent is tetrahydrofuran. The dosage is twice the mass of n-butyric acid.

[0025] The reaction temperature was 60-65°C, and the reaction was carried out for 6 hours. After the reaction was completed, the solvent was evaporated under normal pressure, and the fraction at 100-110°C was collected by distillation to obtain 94.3g of n-butyryl chloride, with a product yield of 88.5% and a purity of 98.5%.

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Abstract

The invention relates to a green chemical synthetic method for n-butyryl chloride, in particular to a chemical synthetic method for preparing n-butyryl chloride by utilizing the reaction between bis (trichloromethyl) carbonate and n-butyric acid. The method comprises the steps of: with n-butyric acid and bis (trichloromethyl) carbonate as the raw materials, reacting in organic solvent at the temperature of 50 DEG C to 100 DEG C for 1 to 10 hours under the action of an organic amine catalyst, and then distilling to obtain the n-butyryl chloride. The method provided by the invention has the advantages of advanced process route, reasonable process conditions, simplicity and safety in operation, high reaction yield rate, low production cost, and less 'three wastes' (waste gas, waste water and waste residues); and the method has greater implementation value and social and economical benefits.

Description

technical field [0001] The invention relates to a green chemical synthesis method of n-butyryl chloride, in particular to a chemical synthesis method for preparing n-butyryl chloride by reacting bis(trichloromethyl)carbonate and n-butyric acid. Background technique [0002] N-butyryl chloride is a colorless and transparent liquid with a boiling point of 98-100°C and a relative density of 1.0263 (20°C). N-butyryl chloride is an important intermediate in organic synthesis, used for the preparation of butyrophenone and uric acid from pharmaceuticals, and the intermediate Body 2-ethyl-1,3-cyclopentanedione, and important raw materials for liquid crystal chemicals and photoinitiators, etc. [0003] Before the present invention was given, the chemical synthesis methods of n-butyryl chloride in the prior art were mostly prepared by n-butyric acid and thionyl chloride or phosphorus oxychloride. Such as "Gansu Chemical Industry" 2006.1 (28) to prepare by reacting 88g (1mol) of n-but...

Claims

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Application Information

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IPC IPC(8): C07C53/42C07C51/60
Inventor 孙敏儿孙燕张松桥陆金明
Owner 湖州沙龙化工有限公司
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