Synthetic method of iodized vegetable fatty acids and their esters

A technology of vegetable oil fatty acid and synthesis method, which is applied in the field of synthesis of iodinated vegetable oil fatty acid and its ester, can solve the problems of unsuitability for industrialized large-scale production, difficulty in removing silicon ether, and high price of trialkylsilyl chloride, and achieves good stability. , low cost, less pain for patients

Inactive Publication Date: 2010-03-24
房新雨
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Problems solved by technology

Although this method is convenient for production and operation, the price of trialkylchlorosilicon is relatively high, and it

Method used

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  • Synthetic method of iodized vegetable fatty acids and their esters

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preparation example Construction

[0019] In conjunction with accompanying drawing, the technical scheme that the present invention adopts is: a kind of synthetic method of iodinated vegetable oil fatty acid and ester thereof, comprises the steps:

[0020] (1) Synthesis of vegetable oil fatty acid: according to the ratio of vegetable oil: sodium hydroxide (or potassium hydroxide): water = 100: 20~100: 100~1000, saponify at 40~110°C for 1~24 hours, and cool to room temperature , filtered to obtain soap powder, and acidified to obtain vegetable oil fatty acid;

[0021] (2) Synthesis of iodinated vegetable oil fatty acid: by vegetable oil fatty acid: hydroiodic acid: the ratio of organic solvent=100: 50~300: 200~1000, iodide 1~96 hours at 0~50 ℃, then reclaim solvent, Add petroleum ether to wash, decolorize, distill and dry to obtain iodized vegetable oil fatty acid;

[0022] (3) Synthesis of iodinated vegetable oil fatty acid ester: by iodinated vegetable oil fatty acid: sulfuric acid: the ratio of alcohol=100: ...

example 1

[0029] Example 1 (synthesis of iodized poppy seed oleic acid and its ethyl ester)

[0030] Ingredients and their sources:

[0031] Poppy seed oil: Plant Oil Factory of Gansu Nongken Medicine and Medicinal Materials Station; Sodium Hydroxide: Jiangyan Reagent Factory, Hedong District, Tianjin; Hydrochloric Acid: Beijing Chemical Plant; Sulfuric acid: Beijing Chemical Plant; Absolute Ethanol: Beijing Chemical Plant; Phosphorus Trichloride : China Tingxin Chemical Reagent Factory; Acetonitrile: Tianjin Yongda Chemical Reagent Development Center; Anhydrous Sodium Iodide: Tianjin Damao Chemical Reagent Factory; Petroleum Ether (60-90): Tianjin Jindong Tianzheng Fine Chemical Reagent Factory ; Silica gel: Qingdao Ocean Chemical Co., Ltd.; Anhydrous sodium sulfate: Tianjin Yongda Chemical Reagent Development Center.

[0032] Put 250g of sodium hydroxide and 1L of water into the reaction bottle, stir and dissolve, add 500g of poppy seed oil, reflux for 3h, cool and filter. Add 100 m...

example 2

[0035] Example 2 (synthesis of methyl iodized corn oleate)

[0036] Ingredients and their sources:

[0037] Corn oil: North China Pharmaceutical Group Kangxin Co., Ltd.; Methanol: Beijing Chemical Plant; other raw materials are the same as Example 1.

[0038] Put 200g of sodium hydroxide and 1L of water into the reaction bottle, stir and dissolve, add 500g of corn oil, react at 95-100°C for 4h, cool, and filter. Add 100 mL of water to the filter cake, heat to 90°C, add hydrochloric acid to pH 1, and stir until the layers are completely separated. Separate layers while hot, wash with hot water, and dry to obtain fatty acids.

[0039]Put 200g fatty acid, 20% sulfuric acid-methanol (v / v) 250mL in the reaction bottle, reflux for 4h, let it stand for stratification, add 200mL of water to the upper layer, adjust the pH to 7~8 with 5% sodium bicarbonate, separate the layers, and the organic layer Wash with water to obtain methyl corn oleate, which is directly used in the next step...

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Abstract

The invention relates to a synthetic method of iodized vegetable fatty acids and their esters. In the invention, at first, vegetable fatty acids are prepared from vegetable oils by the saponificationand acidification, the fatty acids are in the iodination reaction with phosphorus trichloride, phosphorous oxychloride or phosphorus pentachloride and alkali metal iodides such as sodium iodide and the like in an organic medium in the presence of water to generate a hydroiodic acid on site. The iodized vegetable fatty acids are reacted with the alcohol in the catalysis of the acid to produce iodized vegetable fatty acid esters.

Description

technical field [0001] The invention relates to a method for synthesizing iodized vegetable oil fatty acid and its ester. technical background [0002] Iodized vegetable oil fatty acid and its ester is a relatively mature drug, commonly known as iodized oil, which has been widely used at home and abroad, and can be used as a contrast agent, iodine supplement and chemical embolism excipient. Iodized oil has been recorded in the Chinese Pharmacopoeia 1990-2005 edition. As an oral iodine supplement, cost reduction is an important factor that can be widely used in iodine-deficient poverty-stricken areas. As an injection for imaging, iodine supplementation and chemical embolism, in addition to the cost factor, the product with low viscosity is more conducive to reducing the pain of patients and enhancing its curative effect. [0003] There have been several patent reports on the technical synthesis of iodized oil. A synthetic method (CN 95111943.5) of edible oil iodine additive...

Claims

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Application Information

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IPC IPC(8): C07C69/003C07C67/03C07C67/307C07C69/58C07C69/52A61K49/04A61K31/21A61P5/14
Inventor 房新雨
Owner 房新雨
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