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Simple synthetic method of isononanoyl chloride

A technology of isononanoyl chloride and a synthesis method, which is applied in the synthesis of acid chloride compounds and the field of synthesis of isononanoyl chloride, can solve the problems of high requirements on reaction conditions, difficult control of environmental pollution, and high corrosiveness of equipment, and achieves high product purity. , easy to store, transport and use, the effect of less three wastes

Inactive Publication Date: 2009-01-21
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the production of isononanoyl chloride is mainly through isononanoic acid and PCl3, PCl5, POCl3, diphosgene and phosgene, etc. These acyl chlorination agents are highly toxic, irritating, dangerous to operate, require high reaction conditions, high cost, highly corrosive to equipment, complicated post-treatment, and difficult to control environmental pollution defect

Method used

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  • Simple synthetic method of isononanoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: in the 50ml four-neck flask that is equipped with thermometer, mechanical stirring, reflux condenser, drying tube and tail gas absorption bottle, at room temperature, under normal pressure, add 4.45g two (trichloromethyl) carbonate solids, Then add 2.37g isononanoic acid and 0.005g morpholine; start stirring, and slowly raise the temperature to 75°C, keep warm, and react until no gas is generated (generally takes about 1 hour); after the reaction solution is cooled, distill under reduced pressure to obtain iso nonanoyl chloride. According to gas chromatography analysis, the yield of isononanoyl chloride is 87.9%, the purity is 98.62%, the appearance is light yellow liquid, b.p.90~92°C / 20kpa.

Embodiment 2

[0015] Embodiment 2: keep the feed ratio of two (trichloromethyl) carbonate solids, isononanoic acid and catalyst morpholine constant, change the solvent added to be chloroform, other operations are all the same as in Example 2, the isononanoyl chloride obtained , analyzed by gas chromatography, the yield of isononanoyl chloride is 77.65%, the purity is 99.32%, the appearance is colorless liquid, b.p.90~92°C / 20kpa.

Embodiment 3

[0016] Embodiment 3: keep the feed ratio of two (trichloromethyl) carbonate solids, isononanoic acid and catalyst morpholine constant, change the solvent that adds is carbon tetrachloride, other operation is all the same as embodiment 2, obtains Isononanoyl chloride, analyzed by gas chromatography, the yield of isononanoyl chloride is 71.1%, the purity is 98.18%, the appearance is colorless liquid, b.p.90~92℃ / 20kpa.

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Abstract

The invention provides a simple method for synthesizing iso-pelargonyl chloride. The method comprises the following steps that bischloromethyl (trichloromethyl) carbonic ester and isononanoic acid are put into a reactor according to a molar ratio of between 1.0 to 3 and 1.5 to 3; organic amine the mass percent of isononanoic acid of which is between 1 and 10 percent is added as a catalyst and is stirred; moreover, temperature increases to 20 to 150 DEG C and the reaction is kept for 20 to 150min; and finally, iso-pelargonyl chloride is obtained through vacuum distillation after cooling. Moreover, after gas chromatographic analysis, the purity of the obtained acyl chloride is more than 99.00 percent and the yield is more than 90.00 percent. The method for preparing iso-pelargonyl chloride has the advantages of advanced technological line, moderate technological conditions, simple and safe operation, high reaction yield, low production cost, less three wastes and byproducts, and higher implementary value and socioeconomic benefits.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and relates to a synthesis method of acid chloride compounds, in particular to a synthesis method of isononanoyl chloride. Background technique [0002] Isononanoyl chloride is an aliphatic acid chloride, the chemical name is 3,5,5-trimethylhexanoyl chloride, the CAS number is 36727-29-4, the English name is Isononanoyl Chloride or 3,5,5-Trimethylhexanoylchloride, and the density is 0.93 Kg / m 3 , with a boiling point of 188-190°C, a refractive index of 1.436, and a flash point of 284°F. It is an important chemical raw material for the production of initiators. At present, the production of isononanoyl chloride is mainly through isononanoic acid and PCl 3 , PCl 5 , POCl 3 , diphosgene and phosgene as the reaction of acyl chloride agents, these acyl chloride agents are highly toxic, irritating, dangerous to operate, require high reaction conditions, high cost, highly corrosive to equipment, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/126C07C51/60
Inventor 张有明陈小春魏太保李景峰
Owner NORTHWEST NORMAL UNIVERSITY
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