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Method for synthesizing oleoyl chloride by triphosgene

A technology of triphosgene and oleoyl chloride, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as low product purity and yield, environmental pollution, and high requirements for equipment conditions, and achieve high yield And the effect of high yield, safe operation, and little environmental pollution

Inactive Publication Date: 2012-10-17
HEFEI UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these production methods have relatively large defects. It not only requires high equipment conditions, but also generates a large number of by-products (such as: phosphorous acid, etc.), and phosphorus trichloride and thionyl chloride are still toxic and harmful. Chemicals, whose residues will cause great pollution to the environment, and the product purity and yield are also low

Method used

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  • Method for synthesizing oleoyl chloride by triphosgene
  • Method for synthesizing oleoyl chloride by triphosgene
  • Method for synthesizing oleoyl chloride by triphosgene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 0.05mol of purified oleic acid and add it to a 250ml three-necked flask. The temperature of the water bath rises to 60°C and remains constant. Add 0.025mol of triphosgene, and then slowly dropwise add 0.77ml of N,N-dimethylformamide. The constant temperature reaction time is set to 2h, after the reaction is completed, stand for 0.5h~1h to separate the upper layer of the mixture. And calculate the purity and yield of the target product.

[0026] Purity / %

Embodiment 2

[0028] Weigh 0.05mol of purified oleic acid and add it to a 250ml three-necked flask. The temperature of the water bath rises to 60°C and remains constant. Add 0.025mol of triphosgene, and then slowly dropwise add 0.77ml of N,N-dimethylformamide. The constant temperature reaction time is set to 0.5h, after the reaction is completed, stand for 0.5h~1h to separate the upper layer of the mixture. And calculate the purity and yield of the target product.

[0029] Purity / %

Embodiment 3

[0031] 0.05mol of purified oleic acid was weighed into a 250ml three-necked flask, the temperature of the water bath was raised to 80°C and kept constant, 0.025mol of triphosgene was added, and then 0.77ml of N,N-dimethylformamide was slowly added dropwise, and the reaction time at constant temperature was 0.5 h, after the reaction is completed, stand for 0.5h~1h to separate the upper layer of the mixture. And calculate the purity and yield of the target product.

[0032] Purity / %

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Abstract

The invention aims to provide a novel method for synthesizing oleoyl chloride, wherein oleic acid and triphosgene are taken as raw materials, N, N-dimethyl formamide is taken as a catalyst, and the oleic acid and triphosgene and the N,N-dimethyl formamide are reacted for 0.5-8h at 40-80 DEG C. The addition of the catalyst is 10-30% of molar weight of oleic acid, and the molar ratio of oleic acid and triphosgene is 3:1-1:1. The method is not only safe and convenient, but also mild in reaction condition, high in purity of product oleoyl chloride and high in yield.

Description

1. Technical field [0001] The invention relates to a novel synthesis method for oleoyl chloride, in particular to a method for synthesizing oleoyl chloride by using oleic acid and triphosgene as raw materials. 2. Background technology [0002] The synthesis of acid chloride takes carboxylic acid and acylating reagent as raw materials for reaction, and the main methods are as follows: phosphorus trichloride method is convenient for preparing low-boiling acid chloride; phosphorus pentachloride method is used for preparing higher-boiling carboxylic acid chloride. The scope is limited and the post-processing of the generated phosphorus-containing compounds is difficult; the reaction conditions for preparing acid chloride by the thionyl chloride method are mild, but the amount of thionyl chloride is large, the production cost is higher, and the equipment is seriously corroded; phosgene The industrial application of phosgene was earlier, but phosgene is a highly toxic gas, which h...

Claims

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Application Information

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IPC IPC(8): C07C57/66C07C51/60
Inventor 柴多里吴杰鲍远志
Owner HEFEI UNIV OF TECH
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